Preparation method of high-crystallinity Fe-based hydrotalcite-like compound

A hydrotalcite and iron-based technology, which is applied in chemical instruments and methods, iron compounds, inorganic chemistry, etc., can solve problems that cannot effectively meet metal ion reaction conditions, limitations, and complex reaction processes, and achieve simple operation and mild process conditions , The effect of simplifying the preparation process

Active Publication Date: 2014-06-18
桑普能源科技有限公司
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  • Abstract
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Problems solved by technology

This may be due to the different pH values ​​required for co-precipitation of different metal ions in the solution. For iron-based hydrotalcites, the alkali source provided by urea decomposition under normal pressure cannot effectively meet the requirements for the co-precipitation of metal ions. Reaction conditions required for precipitation
Although Huang Yan et al. synthesized magnesium-iron-based anionic layered mater

Method used

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  • Preparation method of high-crystallinity Fe-based hydrotalcite-like compound
  • Preparation method of high-crystallinity Fe-based hydrotalcite-like compound
  • Preparation method of high-crystallinity Fe-based hydrotalcite-like compound

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Experimental program
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Embodiment 1

[0025] The preparation of embodiment 1 nickel-iron-based hydrotalcite

[0026] Step A: 5.4527g (0.0189mol) of solid Ni(NO 3 ) 2 ·6H 2 O and 2.5250g (0.0063mol) of solid Fe(NO 3 ) 3 9H 2 O is dissolved in 50ml deionized water, and stirred to make it dissolve to obtain a mixed solution, the total metal ion concentration (Ni 2+ +Fe 3+ ) is 0.5mol / L, and the molar ratio of nickel and iron ions is 3:1.

[0027] Step B: Add 17.0270 g (0.2835 mol) of urea to the mixed solution obtained in Step A, the molar concentration ratio of urea to nitrate ions in the mixed solution is 5:1, stir for 3-5 minutes until the urea is completely dissolved in the mixed solution .

[0028] Step C: Transfer the mixed solution added with urea to a polytetrafluoroethylene liner of a 100ml hydrothermal synthesis reactor, tighten the reactor and place it in an oven. The hydrothermal reaction was carried out at 90° C., and the reaction time was 72 hours. After the reaction is completed, the reaction...

Embodiment 2

[0032] The preparation of embodiment 2 nickel-iron-based hydrotalcites

[0033] Step A: 5.4527g (0.0189mol) of solid Ni(NO 3 ) 2 ·6H 2 O and 2.5250g (0.0063mol) of solid Fe(NO 3 ) 3 9H 2 O is dissolved in 25ml deionized water, stirred to make it dissolve to obtain a mixed solution, the total metal ion concentration (Ni 2+ +Fe 3+ ) is 1.0mol / L, and the molar ratio of nickel and iron ions is 3:1.

[0034] Step B: Add urea-27.2432g (0.4536mol) to the mixed solution obtained in step A, the molar concentration ratio of urea to nitrate ions in the mixed solution is 8:1, stir for 3-5 minutes until the urea is completely dissolved in the mixed solution middle.

[0035] Step C: Transfer the mixed solution added with urea to a polytetrafluoroethylene liner of a 100ml hydrothermal synthesis reactor, tighten the reactor and place it in an oven. The hydrothermal reaction was carried out at 120° C., and the reaction time was 48 hours. After the reaction is completed, the reaction ...

Embodiment 3

[0037] The preparation of embodiment 3 nickel-iron-based hydrotalcites

[0038] Step A: 3.6351g (0.0126mol) of solid Ni(NO 3 ) 2 ·6H 2 O and 2.5250g (0.0063mol) of solid Fe(NO 3 ) 3 9H 2 O is dissolved in 100ml deionized water, stirred to make it dissolve to obtain a mixed solution, the total metal ion concentration (Ni 2+ +Fe 3+ ) is 0.25mol / L, and the molar ratio of nickel and iron ions is 2:1.

[0039] Step B: Add 10.2162 g (0.1701 mol) of urea to the mixed solution obtained in Step A, the molar concentration ratio of urea to nitrate ions in the mixed solution is 3:1, stir for 3-5 minutes until the urea is completely dissolved in the mixed solution .

[0040] Step C: Transfer the mixed solution added with urea to a polytetrafluoroethylene liner of a 200ml hydrothermal synthesis reactor, tighten the reactor and place it in an oven. The hydrothermal reaction was carried out at 80° C., and the reaction time was 60 hours. After the reaction is completed, the reaction ...

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Abstract

The invention relates to a preparation method of a Fe-based hydrotalcite-like compound, and the preparation method is as follows: first preparing a divalent metal M salt and trivalent Fe salt mixed solution, adding urea to the mixed solution, stirring until the salts are dissolved, and then reacting at 80-120 DEG C in a closed environment for 24 to 96 hours to obtain the Fe-based hydrotalcite-like compound; wherein metal M is selected from the group consisting of Ni, Mg or Co. According to the preparation method, the characteristic of uniform interior pH of the solution of an urea method, the high-crystallinity uniform-size hydrotalcite-like compound can be prepared, the preparation process of the Fe-based hydrotalcite-like compound can be simplified, the ratio of divalent and trivalent metallic element can be controllably adjusted in a certain range. The preparation method of the invention is one-step in reaction, low in cost, simple in operation, mild in reaction conditions, and in favor of further preparation of the Fe-based hydrotalcite-like compound into a thin film and a device.

Description

technical field [0001] The invention relates to the field of inorganic materials, in particular to a method for preparing iron-based hydrotalcites with high crystallinity by a urea method. Background technique [0002] Anionic layered inorganic functional materials are also called hydrotalcite-like (LDHs), the element composition of the main layer, and the type and quantity of the guest anion between the layers are all adjustable. These characteristics make LDHs have a variety of excellent physical and chemical properties, showing extremely broad application prospects in the fields of catalysis, adsorption, separation, ceramic material precursors, photoelectric and photochemical reaction media, and biological nanomaterials. The introduction of nickel and ferromagnetic transition metal elements at the same time greatly facilitates the expansion of its application range in the fields of light, electricity, and magnetism. As an important index parameter, the particle size dist...

Claims

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Application Information

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IPC IPC(8): C01G53/00C01G51/00C01G49/00
Inventor 张英超
Owner 桑普能源科技有限公司
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