CN114634209A - Method for preparing iron oxide red by using ferrous sulfate - Google Patents
Method for preparing iron oxide red by using ferrous sulfate Download PDFInfo
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- CN114634209A CN114634209A CN202210185964.2A CN202210185964A CN114634209A CN 114634209 A CN114634209 A CN 114634209A CN 202210185964 A CN202210185964 A CN 202210185964A CN 114634209 A CN114634209 A CN 114634209A
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 178
- 239000011790 ferrous sulphate Substances 0.000 title claims abstract description 53
- 235000003891 ferrous sulphate Nutrition 0.000 title claims abstract description 53
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 title claims abstract description 53
- 229910000359 iron(II) sulfate Inorganic materials 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 42
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 60
- 238000006243 chemical reaction Methods 0.000 claims abstract description 31
- 239000013078 crystal Substances 0.000 claims abstract description 29
- 238000005273 aeration Methods 0.000 claims abstract description 20
- 239000002244 precipitate Substances 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 3
- 239000000047 product Substances 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 abstract description 12
- 230000008901 benefit Effects 0.000 abstract description 10
- 230000003647 oxidation Effects 0.000 abstract description 10
- 238000007254 oxidation reaction Methods 0.000 abstract description 10
- 230000015572 biosynthetic process Effects 0.000 abstract description 5
- 239000012295 chemical reaction liquid Substances 0.000 abstract description 5
- 238000003786 synthesis reaction Methods 0.000 abstract description 5
- 239000002351 wastewater Substances 0.000 abstract description 5
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 abstract description 4
- 229910001448 ferrous ion Inorganic materials 0.000 abstract description 4
- 239000000243 solution Substances 0.000 description 25
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 17
- 239000011259 mixed solution Substances 0.000 description 13
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 8
- 229910052742 iron Inorganic materials 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 230000008569 process Effects 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000001354 calcination Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000002912 waste gas Substances 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- MMDJDBSEMBIJBB-UHFFFAOYSA-N [O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[NH6+3] Chemical compound [O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[NH6+3] MMDJDBSEMBIJBB-UHFFFAOYSA-N 0.000 description 2
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- XOFYZVNMUHMLCC-ZPOLXVRWSA-N prednisone Chemical compound O=C1C=C[C@]2(C)[C@H]3C(=O)C[C@](C)([C@@](CC4)(O)C(=O)CO)[C@@H]4[C@@H]3CCC2=C1 XOFYZVNMUHMLCC-ZPOLXVRWSA-N 0.000 description 2
- 239000002910 solid waste Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 238000004065 wastewater treatment Methods 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 239000001023 inorganic pigment Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052603 melanterite Inorganic materials 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 229910003145 α-Fe2O3 Inorganic materials 0.000 description 1
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- 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
- C01G49/06—Ferric oxide [Fe2O3]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Iron (AREA)
Abstract
The invention discloses a method for preparing iron oxide red by using ferrous sulfate, which comprises the following steps: mixing a sodium hydroxide solution and a ferrous sulfate solution according to the molar ratio of ferrous sulfate to sodium hydroxide of 1: 3-3: 1, controlling the pH value of a reaction system to be 8-11, and carrying out an aeration reaction to obtain iron oxide red seed crystals; mixing a ferrous sulfate solution and iron oxide red seed crystals according to the molar ratio (0.3-0.8) of ferrous sulfate to iron oxide red seed crystals of 1, adjusting the initial pH value of a reaction system to 7-10 for the first time, stirring and reacting at 60-90 ℃ for 6-12 hours, and then preparing iron oxide red precipitate. The method has the outstanding advantages that the oxidation time in the seed crystal preparation process is short, the iron oxide red seed crystal can be prepared within 2 hours, and the preparation efficiency is high. In the oxidation synthesis stage, the pH value of the reaction liquid is adjusted once, the time for producing the iron oxide red is within 12 hours, the preparation time is greatly shortened, no ferrous ions exist in the reaction liquid, and the treatment difficulty of subsequent wastewater is reduced.
Description
Technical Field
The invention relates to a method for preparing iron oxide red by using ferrous sulfate.
Background
Ferrous sulfate is an industrial solid waste discharged in the production of titanium dioxide by a sulfuric acid method, and the chemical composition of the ferrous sulfate is FeSO4·7H2O cannot be directly used because it contains many impurities. At present, only part of ferrous sulfate is refined and utilized, and the rest isAll are disposed of in a stockpiling mode, which not only has influence on the environment, but also causes waste of iron resources.
Iron oxide red is also called iron oxide red and has a chemical formula of alpha-Fe2O3It is an inorganic pigment with wide application. The iron oxide red has high coloring strength, acid and alkali resistance, high purity and good thermal stability, and is widely applied to the fields of magnetic materials, coatings, catalysis, biomedicine and the like.
At present, the preparation method of iron oxide red can be divided into two main categories, namely a dry method and a wet method. The dry process mainly comprises a ferrous sulfate calcining method, an iron oxide yellow calcining method and an iron oxide black calcining method; the wet process mainly comprises a nitric acid method, a sulfuric acid method and a mixed acid method.
In the technical method, the calcination temperature of the dry process is high, so that the energy consumption is high, meanwhile, the high-temperature calcination is easy to cause crystal agglomeration, and the obtained material has poor dispersibility and influences the quality of the iron oxide red. Nitrogen oxide waste gas and acid waste water are generated in the wet process production, the environmental problem is prominent, and the requirements of clean production are not met.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide the preparation method of the iron oxide red, which has the advantages of low cost, low energy consumption, easy large-scale production, short reaction time, capability of avoiding the pollution of ammonia nitrogen, nitrate nitrogen wastewater, nitric oxide waste gas and the like and excellent product performance. The invention only takes the industrial solid waste ferrous sulfate as an iron source, and prepares the iron oxide red by using an air oxidation method, the ferrous sulfate has high utilization rate, and the iron oxide red has good economic benefit and environmental benefit, and simultaneously, the prepared iron oxide red has high quality, the purity is more than 96 percent, and the iron oxide red reaches the technical requirements of GB1863-2008 products.
The purpose of the invention is realized by the following technical scheme:
a method of preparing iron oxide red comprising the steps of:
(1) mixing a sodium hydroxide solution and a ferrous sulfate solution according to the molar ratio of ferrous sulfate to sodium hydroxide of 1: 3-3: 1, controlling the pH value of a reaction system to be 8-11, and carrying out an aeration reaction to obtain iron oxide red seed crystals;
(2) mixing a ferrous sulfate solution and iron oxide red seed crystals according to a molar ratio (0.3-0.8) of 1, adjusting the initial pH value of a reaction system to 7-10 for the first time, and stirring and reacting at 60-90 ℃ for 6-12 hours to obtain iron oxide red precipitate;
preferably, the concentration of the ferrous sulfate solution is 0.5-1 mol/L, and the concentration of the sodium hydroxide solution is 0.5-3 mol/L;
carrying out the aeration reaction in the step (1), wherein the aeration time is 30 min-2 h;
after the iron oxide red precipitate is prepared in the step (2), filtering, washing, drying and grinding the precipitate to prepare an iron oxide red product;
the drying is preferably carried out at 105 ℃.
Compared with the prior art, the invention has the following advantages and effects:
(1) compared with the production mode of wet preparation and iron sheet, the method has the advantages that the raw material cost is high, the industrial waste ferrous sulfate is only used as an iron source, the air oxidation aeration cost is low, and the prepared iron oxide red has good economic benefit and environmental benefit.
(2) Compared with the prior art for preparing the iron oxide red under a low-temperature system, the method disclosed by the invention has the advantages that the problems of high energy consumption, serious secondary pollution caused by ammonia nitrogen, nitrate nitrogen wastewater, nitrogen oxide waste gas and the like in a wet process are avoided, the process flow is simple and convenient, and the method is suitable for large-scale industrial application.
(3) The method has the outstanding advantages that the oxidation time in the seed crystal preparation process is short, the iron oxide red seed crystal can be prepared within 2 hours, and the preparation efficiency is high. In the oxidation synthesis stage, the pH value of the reaction liquid is adjusted once, the time for producing the iron oxide red is within 12 hours, the preparation time is greatly shortened, no ferrous ions exist in the reaction liquid, and the treatment difficulty of subsequent wastewater is reduced.
(4) The iron oxide red produced by the method has high quality, is bright red, has the purity of over 96 percent, and meets the technical requirements of GB1863-2008 products.
Drawings
FIG. 1 is an XRD pattern of iron oxide red obtained in examples 1-4.
FIG. 2 is an SEM photograph of the iron oxide red obtained in example 3.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited thereto.
Example 1
A method of preparing iron oxide red comprising the steps of:
(1) dropwise adding a ferrous sulfate solution (containing 0.1mol of ferrous sulfate) and a sodium hydroxide solution (containing 0.2mol of sodium hydroxide) into the reactor, carrying out aeration while dropwise adding, and simultaneously controlling the pH value of the reaction system to be 8 and the aeration time to be 2 hours to prepare the iron oxide red seed crystal.
(2) Mixing a ferrous sulfate solution (containing 0.03mol of ferrous sulfate) and 0.1mol of iron oxide red seed crystal, adjusting the pH value of the mixed solution to be 7, placing the mixed solution in a stirrer, setting the reaction temperature to be 80 ℃, and reacting for 12 hours to obtain a precipitate.
(3) And filtering the obtained iron oxide red precipitate, washing, drying at 105 ℃, and grinding to obtain an iron oxide red product.
Example 2
A method of preparing iron oxide red comprising the steps of:
(1) dropwise adding a ferrous sulfate solution (containing 0.1mol of ferrous sulfate) and a sodium hydroxide solution (containing 0.2mol of sodium hydroxide) into the reactor, carrying out aeration while dropwise adding, and simultaneously controlling the pH value of the reaction system to be 9 and the aeration time to be 1 hour to prepare the iron oxide red seed crystal.
(2) Mixing a ferrous sulfate solution (containing 0.05mol of ferrous sulfate) and 0.1mol of iron oxide red seed crystal, adjusting the pH value of the mixed solution to be 8, placing the mixed solution in a magnetic stirrer, setting the reaction temperature to be 80 ℃, and reacting for 10 hours to obtain a precipitate.
(3) And filtering the obtained iron oxide red precipitate, washing, drying at 105 ℃, and grinding to obtain an iron oxide red product.
Example 3
A method of preparing iron oxide red comprising the steps of:
(1) dropwise adding a ferrous sulfate solution (containing 0.1mol of ferrous sulfate) and a sodium hydroxide solution (containing 0.3mol of sodium hydroxide) into the reactor, carrying out aeration while dropwise adding, and simultaneously controlling the pH value of the reaction system to be 10 and the aeration time to be 45min to prepare the iron oxide red seed crystal.
(2) Mixing ferrous sulfate solution (containing 0.06mol of ferrous sulfate) and 0.1mol of iron oxide red seed crystal, adjusting the pH value of the mixed solution to 9, placing the mixed solution in a magnetic stirrer, setting the reaction temperature to 90 ℃, and reacting for 8 hours to obtain precipitate.
(3) And filtering the obtained iron oxide red precipitate, washing, drying at 105 ℃, and grinding to obtain an iron oxide red product.
Example 4
A method of preparing iron oxide red comprising the steps of:
(1) dropwise adding a ferrous sulfate solution (containing 0.1mol of ferrous sulfate) and a sodium hydroxide solution (containing 0.3mol of sodium hydroxide) into the reactor, carrying out aeration while dropwise adding, and simultaneously controlling the pH value of the reaction system to be 11 and the aeration time to be 30min to prepare the iron oxide red seed crystal.
(2) Mixing a ferrous sulfate solution (containing 0.08mol of ferrous sulfate) and 0.1mol of iron oxide red seed crystal, adjusting the pH value of the mixed solution to 10, placing the mixed solution in a magnetic stirrer, setting the reaction temperature to 90 ℃, and reacting for 6 hours to obtain a precipitate.
(3) And filtering the obtained iron oxide red precipitate, washing, drying at 105 ℃, and grinding to obtain an iron oxide red product.
Comparative example 1 (different from the examples in that the pH value in step (3) is 4)
A method of preparing iron oxide red comprising the steps of:
(1) dropwise adding a ferrous sulfate solution (containing 0.1mol of ferrous sulfate) and a sodium hydroxide solution (containing 0.2mol of sodium hydroxide) into the reactor, carrying out aeration while dropwise adding, and simultaneously controlling the pH value of the reaction system to be 8 and the aeration time to be 2 hours to prepare the iron oxide red seed crystal.
(2) Mixing ferrous sulfate solution (containing 0.02mol of ferrous sulfate) and 0.1mol of iron oxide red seed crystal, maintaining the pH value of the mixed solution to be 4, placing the mixed solution in a magnetic stirrer, setting the reaction temperature to be 90 ℃, and reacting for 12 hours to obtain precipitate.
(3) And filtering the obtained iron oxide red precipitate, washing, drying at 105 ℃, and grinding to obtain an iron oxide red product.
Comparative example 2 (different from the example in that the molar ratio of ferrous sulfate to iron oxide red seed crystal in step (3) is 1:1)
A method of preparing iron oxide red comprising the steps of:
(1) dropwise adding a ferrous sulfate solution (containing 0.1mol of ferrous sulfate) and a sodium hydroxide solution (containing 0.2mol of sodium hydroxide) into the reactor, carrying out aeration while dropwise adding, and simultaneously controlling the pH value of the reaction system to be 9 and the aeration time to be 1 hour to prepare the iron oxide red seed crystal.
(2) Mixing ferrous sulfate solution (containing 0.1mol of ferrous sulfate) and 0.1mol of iron oxide red seed crystal, adjusting the pH value of the mixed solution to 10, placing the mixed solution in a magnetic stirrer, setting the reaction temperature to 90 ℃, and reacting for 12 hours to obtain precipitate.
(3) And filtering the obtained iron oxide red precipitate, washing, drying at 105 ℃, and grinding to obtain an iron oxide red product.
As can be seen from FIG. 1, the iron oxide red prepared in examples 1 to 4 has stronger characteristic peaks at 24.2 °, 35.7 °, 40.9 °, 49.5 °, 54.1 °, 62.5 ° and 64.1 °, and is similar to Fe in standard card2O3(PDF73-2234) has consistent diffraction peaks, sharp and symmetrical peak shapes and no impurity peak, and proves that the phase composition of the product prepared by the method is Fe with good crystallinity2O3。
As can be seen from FIG. 2, the sample of iron oxide red prepared in example 3 has a uniform size, a clear edge, and relatively regular particles.
The iron oxide red products obtained in examples 1 to 4 are subjected to technical index analysis, and as shown in the results in table 1, the iron oxide red series indexes prepared by the method all reach the technical requirements of GB1863-2008 first-grade products.
The iron oxide red prepared in examples 1 to 4 and comparative examples 1 to 2 was used in color brightness (L) with a standard sample Bayer iron oxide red RIO sold on the market*) And the color red-yellow (a)*、b*) Are compared above and subjected to color difference (. DELTA.E)*) Calculation of Δ E*If the numerical value of (b) is in the range of 0 to 5, it means that the color difference is small and the colors are similar, and the results are shown in table 2.
As can be seen from table 2, by adjusting the molar ratio of ferrous sulfate to the iron oxide red seed crystal and the pH range in the oxidation synthesis process, the color difference values of the iron oxide red prepared in examples 1 to 4 and the bayer product are respectively 1.49, 4.56, 1.18, and 1.8, and the color difference values are small, which indicates that the iron oxide red prepared by the method has excellent brightness and red hue. In the two-step oxidation stage, ferrous sulfate can catalyze iron oxide red seed crystal to dissolve and recrystallize, the molar ratio is changed in the invention range, and a series of iron oxide red with different red color gradients can be obtained by quantitatively controlling reaction conditions, thereby meeting the actual industrial requirements. Iron oxide red obtained in a molar ratio range which is not within the invention has dark color, iron yellow or iron brown and the like can be obtained, and qualified iron oxide red cannot be prepared.
Comparative example 1 in the oxidation synthesis stage, 0.02mol of ferrous sulfate and 0.1mol of iron oxide red seed crystal were mixed, the pH of the reaction solution was maintained at 4, and after reaction at 90 ℃ for 12 hours, a precipitate was obtained, the pH being lower than the preparation conditions required by the present invention. Under an acidic system with the pH value of 4, ferrous sulfate is not easy to oxidize, a large amount of unoxidized ferrous ions still exist in the reaction liquid after the reaction is finished, so that iron resources are wasted, and the subsequent wastewater treatment cost is higher; the product turns yellow after being dried and ground, the color difference with the standard sample is 16.93, and the iron oxide red obtained under the condition has poor quality. In the preparation process, the pH value of the mixed solution is adjusted to 7-10 in one step, so that the reaction process is accelerated, and the product with excellent red color and brightness can be prepared within 12 hours. After the reaction is finished, sampling liquid is taken, and K is dripped3[Fe(CN)6]The solution does not change color, which indicates that no ferrous ion exists in the system after the reaction is finished, thereby reducing the difficulty of wastewater treatment and ensuring that the reaction process is clean and pollution-free.
In the comparative example 2, the preparation conditions in the oxidation synthesis stage are higher than the molar ratio in the range of the invention, and the prepared product is purple and black, has large color difference with the standard sample, and seriously influences the brightness and the red tone value of the product.
Table 1 analysis results of technical indexes of iron oxide red products obtained in examples
TABLE 2 comparison of iron oxide Red prepared in examples and comparative examples with respect to CIE color values
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (6)
1. A method for preparing iron oxide red is characterized by comprising the following steps:
(1) mixing a sodium hydroxide solution and a ferrous sulfate solution according to the molar ratio of ferrous sulfate to sodium hydroxide of 1: 3-3: 1, controlling the pH value of a reaction system to be 8-11, and carrying out an aeration reaction to obtain iron oxide red seed crystals;
(2) mixing a ferrous sulfate solution and iron oxide red seed crystals according to the molar ratio of ferrous sulfate to iron oxide red seed crystals (0.3-0.8): 1, adjusting the initial pH value of a reaction system to 7-10 for the first time, and stirring and reacting at 60-90 ℃ for 6-12 hours to obtain iron oxide red precipitate.
2. The method of claim 1, wherein: the concentration of the ferrous sulfate solution is 0.5-1 mol/L.
3. The method of claim 1, wherein: the concentration of the sodium hydroxide solution is 0.5-3 mol/L.
4. The method of claim 1, wherein: and (2) carrying out aeration reaction in the step (1), wherein the aeration time is 30 min-2 h.
5. The method of claim 1, wherein: and (3) after the iron oxide red precipitate is prepared in the step (2), filtering, washing, drying and grinding the precipitate to prepare an iron oxide red product.
6. The method of claim 5, wherein: the drying is carried out at 105 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210185964.2A CN114634209B (en) | 2022-02-28 | Method for preparing iron oxide red by using ferrous sulfate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210185964.2A CN114634209B (en) | 2022-02-28 | Method for preparing iron oxide red by using ferrous sulfate |
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| Publication Number | Publication Date |
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| CN114634209A true CN114634209A (en) | 2022-06-17 |
| CN114634209B CN114634209B (en) | 2024-06-04 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4256723A (en) * | 1979-05-03 | 1981-03-17 | Cities Service Company | Process for preparing precipitated red iron oxides |
| US4753680A (en) * | 1985-01-09 | 1988-06-28 | Bayer Aktiengesellschaft | Process for the preparation of bright, color-pure iron oxide red pigments |
| CN1766005A (en) * | 2005-08-23 | 2006-05-03 | 奚长生 | Method for preparing high purity iron oxide yellow and iron oxide red using titanium dioxide byproduct ferrous sulfate |
| CN102557226A (en) * | 2011-12-30 | 2012-07-11 | 华南理工大学 | Production method for preparing iron oxide red seed crystal by using ferrite-containing waste water |
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4256723A (en) * | 1979-05-03 | 1981-03-17 | Cities Service Company | Process for preparing precipitated red iron oxides |
| US4753680A (en) * | 1985-01-09 | 1988-06-28 | Bayer Aktiengesellschaft | Process for the preparation of bright, color-pure iron oxide red pigments |
| CN1766005A (en) * | 2005-08-23 | 2006-05-03 | 奚长生 | Method for preparing high purity iron oxide yellow and iron oxide red using titanium dioxide byproduct ferrous sulfate |
| CN102557226A (en) * | 2011-12-30 | 2012-07-11 | 华南理工大学 | Production method for preparing iron oxide red seed crystal by using ferrite-containing waste water |
Non-Patent Citations (2)
| Title |
|---|
| 佘宗华等: ""用硫酸亚铁全液相合成颜料铁红的研究"", pages 44 - 47 * |
| 赵丽艳: ""δ-FeOOH为晶种制备超细α-Fe2O3及机理研究"", 《CNKI中国知网》, pages 6 - 10 * |
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