Preparation method of ferric oxide

By mixing the iron tetraoxide powder with a catalyst and an oxidant, and reacting it in the alkali solution, the problem of low yield of iron tetraoxide in the prior art is solved, an efficient and green preparation process is achieved, and the yield of iron tetraoxide is significantly improved.

CN119797441APending Publication Date: 2025-04-11HEBEI SAI QIANG METALLURGICAL HEAVY IND MASCH CO LTD
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Patent Information

Application Number
CN202510035568.5
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-01-09
Publication Date
2025-04-11

AI Technical Summary

Technical Problem

In the prior art, the yield of iron dioxide from iron tetroxide is not high, and it is difficult to meet the needs of efficient and green preparation.

Method used

The crude iron trioxide product is prepared by roasting a mixture of iron tetraoxide powder, water, catalyst and oxidizing agent, and reacting, filtering and drying by adding alkali liquid to finally obtain high yield iron trioxide. Among them, titanium dioxide and copper oxide are used as catalysts, manganese dioxide is used as oxidizing agents, and alkali liquid includes aqueous sodium hydroxide solution and ammonia water.

Benefits of technology

By adjusting the mass ratio of the catalyst and oxidant, as well as zinc-doped manganese dioxide, the yield of iron dioxide is significantly improved, achieving an efficient and green preparation process.

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Abstract

The invention relates to the technical field of metal oxide materials, and provides a preparation method of ferric oxide, which comprises the following steps: S1, mixing ferroferric oxide powder, water, a catalyst and an oxidizing agent to obtain a mixture; s2, roasting the mixture to obtain a ferric oxide crude product; s3, adding the ferric oxide crude product into alkali liquor, uniformly mixing, reacting, filtering and drying to obtain ferric oxide; the catalyst comprises titanium dioxide and copper oxide; the oxidant comprises manganese dioxide; the alkali liquor comprises a sodium hydroxide aqueous solution and ammonia water. According to the technical scheme, the problem that the yield of ferric oxide prepared from ferroferric oxide in the prior art is not high is solved.
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Description

Technical Field

[0001] The invention relates to the technical field of metal oxide materials, and in particular to a method for preparing ferric oxide. Background Art

[0002] Ferric oxide, the main component of common rust, has extensive and critical applications in many fields. In the pigment industry, it gives rich and stable colors to products such as coatings and inks with its unique color, and is an important basis for high-quality pigments; in the field of magnetic materials, specially treated ferric oxide can be used as a key component of magnetic recording materials to facilitate accurate storage and reading of information; in the field of environmental protection, it can be used as a catalyst carrier to participate in sewage treatment, waste gas purification and other processes, promoting the advancement of environmental purification technology.

[0003] Ferroferric oxide is also an important iron oxide. It exists naturally in magnetite and has ferromagnetism. It performs well in magnetic devices, electromagnetic shielding materials, etc. However, under some specific needs, ferroferric oxide needs to be converted into ferrous oxide. On the one hand, from the perspective of product performance optimization, for example, when preparing certain fine pigments, ferrous oxide can provide purer and brighter colors than ferrous oxide, meeting the high-end market's stringent requirements for color accuracy; on the other hand, in some chemical reaction systems or material synthesis pathways, subsequent steps may be more suitable for ferrous oxide as a raw material form to ensure the continuity and efficiency of the entire process.

[0004] With the rapid development of materials science and chemical engineering technology, as well as the continuous increase in demand for high-quality ferric oxide in various industries, it is urgent to develop a new, efficient and green technology for preparing ferric oxide from ferroferric oxide. The existing technology for preparing ferric oxide from ferroferric oxide still has the problem of low yield. Therefore, it is very important to develop a high-yield technology for preparing ferric oxide from ferroferric oxide. Summary of the invention

[0005] The invention provides a method for preparing ferric oxide, which solves the problem of low yield of preparing ferric oxide from ferroferric oxide in the related art.

[0006] The technical solution of the present invention is as follows: The present invention provides a method for preparing ferric oxide, comprising the following steps: S1, mixing ferroferric oxide powder, water, a catalyst and an oxidant to obtain a mixture; S2, roasting the mixture to obtain a crude ferric oxide product; S3, adding the crude ferric oxide to an alkali solution, mixing evenly, reacting, filtering, and drying to obtain the ferric oxide; The catalyst includes titanium dioxide and copper oxide; The oxidant includes manganese dioxide; The alkali solution includes sodium hydroxide aqueous solution and ammonia water.

[0007] As a further technical solution, the raw materials include the following components by weight: 100-150 parts of ferroferric oxide powder, 15-25 parts of water, 2-8 parts of catalyst, 3-8 parts of oxidant, and 30-40 parts of alkali solution.

[0008] As a further technical solution, the calcination temperature is 400-600° C. and the calcination time is 4-6 hours.

[0009] As a further technical solution, the concentration of the sodium hydroxide aqueous solution is 0.01 mol / L, the concentration of the ammonia water is 0.01 mol / L, and the mass ratio of the sodium hydroxide aqueous solution to the ammonia water is 2-4:1.

[0010] As a further technical solution, the reaction temperature is 20-30°C and the reaction time is 1-3h.

[0011] As a further technical solution, the mass ratio of titanium dioxide to copper oxide is 2~6:1.

[0012] In the present invention, the mass ratio of titanium dioxide to copper oxide is adjusted to 2-6:1, thereby further improving the yield of ferric oxide.

[0013] As a further technical solution, the manganese dioxide is zinc-doped manganese dioxide.

[0014] As a further technical solution, the preparation process of the zinc-doped manganese dioxide comprises the following steps: mixing zinc powder and manganese dioxide powder, and calcining to obtain the zinc-doped manganese dioxide powder; the calcining temperature is 400-500°C.

[0015] In the present invention, zinc is doped into manganese dioxide to further improve the yield of ferric oxide.

[0016] As a further technical solution, in the zinc-doped manganese dioxide, the mass ratio of manganese dioxide to zinc is 5-9:1.

[0017] In the present invention, the mass ratio of manganese dioxide to zinc in zinc-doped manganese dioxide is adjusted to 5-9:1, thereby further improving the yield of ferric oxide.

[0018] As a further technical solution, the particle size of the ferrosoferric oxide is 200-300 nm.

[0019] As a further technical solution, the particle size of the ferric oxide is 150-250 nm.

[0020] The working principle and beneficial effects of the present invention are: In the present invention, titanium dioxide and copper oxide are used as catalysts to reduce the activation energy of the oxidation reaction, and titanium dioxide and copper oxide act synergistically to improve the yield of preparing ferric oxide. Manganese dioxide is added to the oxidant to promote the occurrence of the oxidation reaction and improve the yield of preparing ferric oxide. The present invention uses alkali solution to remove the catalyst and oxidant in the crude ferric oxide, thereby improving the yield of preparing ferric oxide. DETAILED DESCRIPTION

[0021] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0022] Example 1 A method for preparing ferric oxide comprises the following steps: S1, mixing 150 parts of ferrosoferric oxide powder, 25 parts of water, 8 parts of catalyst, and 8 parts of oxidant to obtain a mixture; S2, calcining the mixture at 600°C for 4 hours to obtain crude ferric oxide; S3, adding the crude ferric oxide to 40 parts of alkali solution, mixing evenly, reacting at 30°C for 1 hour, filtering, and drying to obtain ferric oxide; The catalyst includes titanium dioxide and copper oxide, and the mass ratio of titanium dioxide to copper oxide is 8:1; The oxidant is manganese dioxide; The alkali solution includes sodium hydroxide aqueous solution and ammonia water, and the mass ratio of the sodium hydroxide aqueous solution to the ammonia water is 4:1.

[0023] Example 2 A method for preparing ferric oxide comprises the following steps: S1, mixing 100 parts of ferroferric oxide powder, 15 parts of water, 2 parts of catalyst, and 3 parts of oxidant to obtain a mixture; S2, calcining the mixture at 400°C for 6 hours to obtain crude ferric oxide; S3, adding the crude ferric oxide to 30 parts of alkali solution, mixing evenly, reacting at 20°C for 3h, filtering, and drying to obtain ferric oxide; The catalyst includes titanium dioxide and copper oxide, and the mass ratio of titanium dioxide to copper oxide is 1:2; The oxidant is manganese dioxide; The alkali solution includes sodium hydroxide aqueous solution and ammonia water, and the mass ratio of the sodium hydroxide aqueous solution to the ammonia water is 2:1.

[0024] Example 3 A method for preparing ferric oxide comprises the following steps: S1, mixing 125 parts of ferrosoferric oxide powder, 20 parts of water, 5 parts of catalyst, and 6 parts of oxidant to obtain a mixture; S2, calcining the mixture at 500°C for 5h to obtain crude ferric oxide; S3, adding the crude ferric oxide to 35 parts of alkali solution, mixing evenly, reacting at 25°C for 2h, filtering, and drying to obtain ferric oxide; The catalyst includes titanium dioxide and copper oxide, and the mass ratio of titanium dioxide to copper oxide is 1:1; The oxidant is manganese dioxide; The alkali solution includes sodium hydroxide aqueous solution and ammonia water, and the mass ratio of the sodium hydroxide aqueous solution to the ammonia water is 3:1.

[0025] Example 4 The only difference between this embodiment and embodiment 3 is that the mass ratio of titanium dioxide to copper oxide in this embodiment is 7:1.

[0026] Example 5 The only difference between this embodiment and embodiment 3 is that the mass ratio of titanium dioxide to copper oxide in this embodiment is 2:1.

[0027] Example 6 The only difference between this embodiment and embodiment 3 is that the mass ratio of titanium dioxide to copper oxide in this embodiment is 4:1.

[0028] Example 7 The only difference between this embodiment and embodiment 3 is that the mass ratio of titanium dioxide to copper oxide in this embodiment is 6:1.

[0029] Example 8 The difference between this embodiment and embodiment 6 is that the oxidant in this embodiment is zinc-doped manganese dioxide, the mass ratio of manganese dioxide to zinc is 12:1, and the preparation process of zinc-doped manganese dioxide includes the following steps: mixing zinc powder and manganese dioxide powder, calcining to obtain zinc-doped manganese dioxide powder; the calcining temperature is 450°C.

[0030] Example 9 The only difference between this embodiment and embodiment 8 is that the mass ratio of manganese dioxide to zinc in this embodiment is 3:1.

[0031] Example 10 The only difference between this embodiment and embodiment 8 is that the mass ratio of manganese dioxide to zinc in this embodiment is 5:1.

[0032] Embodiment 11 The only difference between this embodiment and embodiment 8 is that the mass ratio of manganese dioxide to zinc in this embodiment is 7:1.

[0033] Example 12 The only difference between this embodiment and embodiment 8 is that the mass ratio of manganese dioxide to zinc in this embodiment is 9:1.

[0034] Comparative Example 1 The only difference between this comparative example and Example 2 is that the catalyst in this comparative example contains only titanium dioxide.

[0035] Comparative Example 2 The difference between this comparative example and Example 2 is that the catalyst in this comparative example contains only copper oxide.

[0036] Comparative Example 3 The only difference between this comparative example and Example 2 is that this comparative example does not contain a catalyst.

[0037] Comparative Example 4 The only difference between this comparative example and Example 2 is that this comparative example does not contain an oxidant.

[0038] The ferric oxide obtained in Examples 1 to 12 and Comparative Examples 1 to 4 was tested as follows: The iron oxide was analyzed by X-ray fluorescence spectrometer to measure the purity of the iron oxide and further obtain the iron oxide yield. The test results are shown in Table 1.

[0039] A=(m×a) / m1; A is the yield of ferric oxide, m is the mass of ferric oxide, a is the purity of ferric oxide measured by X-ray fluorescence spectrometer analysis, and m1 is the mass of ferric oxide powder.

[0040] Table 1 Test results of purity and yield of ferric oxide

[0041] Comparing Example 2 with Comparative Examples 1 to 3, it is shown that the use of titanium dioxide and copper oxide as catalysts in the present invention produces a synergistic effect and improves the yield of ferric oxide. Comparing Example 2 with Comparative Example 4, it is shown that the use of manganese dioxide as an oxidant in the present invention improves the yield of ferric oxide.

[0042] Comparing Examples 5 to 7 with Examples 3 to 4, it is shown that when the mass ratio of titanium dioxide to copper oxide is adjusted to 2 to 6:1 in the present invention, the yield of ferric oxide is further improved; comparing Example 6 with Examples 5 and 7, it is shown that when the mass ratio of titanium oxide to copper oxide is 4:1, the yield of ferric oxide is further improved. Comparing Examples 8 to 12 with Example 6, it is shown that the use of zinc-doped manganese dioxide in the present invention further improves the yield of ferric oxide; comparing Examples 10 to 12 with Examples 8 to 9, it is shown that when the mass ratio of manganese dioxide to zinc in the zinc-doped manganese dioxide of the present invention is 5 to 9:1, the yield of ferric oxide is further improved; comparing Example 11 with Examples 10 and 12, it is shown that when the mass ratio of manganese dioxide to zinc in the zinc-doped manganese dioxide of the present invention is 7:1, the yield of ferric oxide is best.

[0043] The above are only preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for preparing ferric oxide, characterized in that: The following steps are involved: S1, mixing ferroferric oxide powder, water, a catalyst and an oxidant to obtain a mixture; S2, roasting the mixture to obtain a crude ferric oxide product; S3, adding the crude ferric oxide to an alkali solution, mixing evenly, reacting, filtering, and drying to obtain the ferric oxide; The catalyst includes titanium dioxide and copper oxide; The oxidant includes manganese dioxide; The alkali solution includes sodium hydroxide aqueous solution and ammonia water.

2. A method for preparing ferric oxide according to claim 1, characterized in that: The raw materials include the following components by weight: 100-150 parts of ferroferric oxide powder, 15-25 parts of water, 2-8 parts of catalyst, 3-8 parts of oxidant and 30-40 parts of alkali solution.

3. A method for preparing ferric oxide according to claim 1, characterized in that: The calcination temperature is 400-600° C. and the calcination time is 4-6 hours.

4. A method for preparing ferric oxide according to claim 1, characterized in that: The concentration of the sodium hydroxide aqueous solution is 0.01 mol / L, the concentration of the ammonia water is 0.01 mol / L, and the mass ratio of the sodium hydroxide aqueous solution to the ammonia water is 2-4:

1.

5. A method for preparing ferric oxide according to claim 1, characterized in that: The reaction temperature is 20-30°C and the reaction time is 1-3h.

6. The method for preparing ferric oxide according to claim 1, characterized in that: The mass ratio of titanium dioxide to copper oxide is 2-6:

1.

7. The method for preparing ferric oxide according to claim 1, characterized in that: The manganese dioxide is zinc-doped manganese dioxide.

8. The method for preparing ferric oxide according to claim 7, characterized in that: In the zinc-doped manganese dioxide, the mass ratio of manganese dioxide to zinc is 5-9:

1.

9. The method for preparing ferric oxide according to claim 1, characterized in that: The particle size of the ferrosoferric oxide is 200-300 nm.

10. The method for preparing ferric oxide according to claim 1, characterized in that: The particle size of the ferric oxide is 150-250 nm.