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Preparation method of ferric oxide with different crystal forms

A technology of iron oxide, crystal form, applied in the direction of iron oxide, iron oxide/hydroxide, nanotechnology for materials and surface science, etc., can solve the problems of controllable regulation, different product morphology and properties, etc. , to achieve the effect of preventing solution coagulation, low equipment requirements, and good antifreeze performance

Inactive Publication Date: 2020-10-27
EAST CHINA UNIV OF SCI & TECH
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Problems solved by technology

Different methods have very different reaction principles, reaction equipment and reaction conditions, resulting in different shapes and properties of the products. Therefore, it is difficult in the prior art to achieve nano-scale production of products through the regulation of specific links in the preparation process. The controllable adjustment of the content of α-iron oxide and γ-iron oxide, so the technical problem that needs to be solved urgently is how to mass produce nano-scale Fe 2 o 3 In the process, the crystal form modulation of nano-iron oxide products is realized through the control of process conditions

Method used

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  • Preparation method of ferric oxide with different crystal forms
  • Preparation method of ferric oxide with different crystal forms

Examples

Experimental program
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Effect test

Embodiment 1

[0036] Preparation of α-Fe 2 O 3 The process is as follows:

[0037] First, 2.54g of anhydrous ferrous chloride was weighed and dissolved in the same beaker containing 60ml of ethylene glycol, and ultrasonically stirred for 10 minutes; then, the solution was transferred to a three-necked flask, and the temperature was maintained in an oil bath under magnetic stirring At -20℃, keep for 1h;

[0038] Dissolve 7.52g of ammonium carbonate in 100ml of prepared deionized water, stir ultrasonically for 5min until the sodium carbonate is completely dissolved, and continue to stand for 30min; then add the ammonium carbonate solution dropwise to the ethyl acetate of ferrous chloride at a rate of 1.2ml / min. In the glycol solution, continue to age the precipitate for 2h after the dropwise addition;

[0039]The liquid precipitation mixture was filtered on a suction filter with 1000 mL of deionized water, and the precipitate was separated and transferred to an oven, and dried at 120 °C fo...

Embodiment 2

[0041] Preparation of Alkali-free γ-Fe 2 O 3 The process is as follows:

[0042] First, 2.54g of anhydrous ferrous chloride was weighed and dissolved in the same beaker containing 60ml of ethylene glycol, and ultrasonically stirred for 10 minutes;

[0043] Then, the solution was transferred to a three-necked flask, and the temperature was maintained at -20 °C in an oil bath under magnetic stirring for 1 h; 8.48 g of sodium carbonate was dissolved in 100 ml of prepared deionized water, and ultrasonically stirred for 5 min until the sodium carbonate was completely Dissolve, continue to stand for 30min; then add the sodium carbonate solution dropwise to the ethylene glycol solution of ferrous chloride at a speed of 1.2ml / min, and continue to age the precipitate for 2h after the dropwise addition;

[0044] Distribute the suspension evenly to 6 centrifuge tubes with a range of 50mL, add deionized water to the 35mL mark, centrifuge at 8000r / min for 5 minutes, separate the supernat...

Embodiment 3

[0047] Preparation of γ-Fe by Cellulose Template Impregnation Method 2 O 3 The process is as follows:

[0048] First, cut the cellulose template into a size of 0.5cm×0.5cm, weigh 1g, and add deionized water dropwise to measure its saturated water absorption;

[0049] Next, dissolve 1.875g of ferric nitrate nonahydrate and 0.256g of potassium nitrate in deionized water equal to its saturated water absorption;

[0050] Then, the prepared nitrate solution was added dropwise to the 1 g cellulose template while stirring, and the stirring was continued for 10 min after the dropwise addition;

[0051] Transfer the impregnated cellulose template into an oven at 120 °C for 10 hours until the water evaporates to dryness;

[0052] The dried precipitate was ground and calcined in an air-vented muffle furnace, raised to 900°C at a heating rate of 10°C / min, and held for 4 hours to obtain γ-Fe 2 O 3 .

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Abstract

The invention relates to a preparation method of ferric oxide with different crystal forms. The preparation method comprises the following steps of: preparing a Fe precursor from Fe salt and an alkaline compound aqueous solution containing alkali metal, and controlling the content of residual alkali metal in the Fe precursor to modulate the content of alpha-Fe2O3 and gamma-Fe2O3 in calcined Fe2O3.Compared with the prior art, the preparation method provided by the invention is simple and easy to implement, a preparation method of nano iron oxide with low raw material cost, simple equipment andcontrollable crystal form is provided, and the defect of uncontrollable crystal form in the prior art is overcome; according to the fact that the proportion of alkali metal contained in Fe2O3 is increased from 0 and the crystal form is gradually changed from alpha to gamma during calcination, crystal form modulation of a nano iron oxide product is achieved through control over technological conditions; meanwhile, preparation raw materials are easy to obtain, environmental pollution is small, and industrialization is possible.

Description

technical field [0001] The invention relates to a preparation method of iron oxide, in particular to a preparation method of iron oxide with different crystal forms. Background technique [0002] As a transition metal oxide, iron oxide is widely used as a catalyst in reactions such as sewage treatment and synthesis gas conversion, and is also one of the important functional materials in inorganic materials. There are various classifications of iron oxides, which can be divided into FeO and Fe according to their valence states. 2 O 3 and Fe 3 O 4 , where Fe 2 O 3 According to the crystal form, it can be divided into α, β and γ types. α-Fe is currently the most studied in the literature 2 O 3 and γ-Fe 2 O 3 . α-Fe 2 O 3 It is the most stable crystal structure, usually reddish-brown. It not only has good corrosion resistance, light resistance, weather resistance, but also has good dispersibility and has significant absorption and shielding effects on ultraviolet ra...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/06B82Y30/00
CPCB82Y30/00C01G49/06C01P2002/72C01P2002/82
Inventor 徐晶徐敏杰曹晨熙杨子旭朱明辉李平韩一帆
Owner EAST CHINA UNIV OF SCI & TECH
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