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Preparation method of multi-level structure magnesium borate hollow microspheres

A hollow microsphere, magnesium borate technology, applied in the direction of borates, boron oxides, nanotechnology, etc., to achieve the effect of complete crystal form, easy operation and high yield

Active Publication Date: 2012-07-04
海宁市黄湾镇资产经营有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is still a lack of a controlled synthesis process for preparing high-crystallinity magnesium borate microspheres with different crystal forms, shapes, and sizes in China.

Method used

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  • Preparation method of multi-level structure magnesium borate hollow microspheres
  • Preparation method of multi-level structure magnesium borate hollow microspheres
  • Preparation method of multi-level structure magnesium borate hollow microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] At room temperature (25°C), weigh 1.0 mmol of magnesium nitrate and dissolve it in 10 ml of distilled water to prepare 10 ml of 0.1 mol / L magnesium nitrate aqueous solution, add 0.5 ml of 1-ethyl-3-methylimidazole ethyl sulfate salt, and stir magnetically for 0.5 h, then add 10ml 0.1mol / L borax aqueous solution dropwise, continue to stir for 2h to obtain a white turbid solution, and age the white turbid solution at a constant temperature of 80°C for 48h. After the aging is completed, a precipitated mixture is obtained, and the precipitated mixture is filtered to obtain a white filter cake, and the white filter cake was washed successively with distilled water and absolute ethanol for 3 times, and the filter cake was dried at 120° C. for 24 h to obtain a white product, i.e., hollow microspheres of magnesium borate with a hierarchical structure. XRD (X-ray diffraction, figure 1 Shown) to detect the composition of magnesium borate as Mg 7 B 4 o 13 ·7H 2 O, its diffracti...

Embodiment 2

[0031]At room temperature, weigh 1.0mmol of magnesium sulfate and dissolve it in 100ml of distilled water to prepare 100ml of 0.01mol / L magnesium sulfate aqueous solution, add 1ml of 1-ethyl-3-methylimidazolium tetrafluoroborate, stir magnetically for 0.5h, and then Add 100ml of 0.10mol / L borax aqueous solution dropwise, continue stirring for 3 hours to obtain a white turbid solution, and age the white turbid solution at a constant temperature of 100°C for 12 hours. After the aging is completed, a precipitated mixture is obtained, and the precipitated mixture is filtered to obtain a white filter cake, and After washing the white filter cake with distilled water and absolute ethanol three times in sequence, the filter cake was dried at 80°C for 24 hours to obtain a white product, which is a hollow microsphere of magnesium borate with a hierarchical structure. The magnesium borate has a microcrystalline structure as detected by XRD. for Mg 7 B 4 o 13 ·7H 2 O, its diffraction ...

Embodiment 3

[0033] At room temperature, weigh 1.0mmol of magnesium chloride and dissolve it in 10ml of distilled water to prepare 10ml of 0.1mol / L magnesium nitrate aqueous solution, add 6ml of 1-ethyl-3-methylimidazole acetate, stir magnetically for 0.5h, and then add dropwise 10ml 0.01mol / L borax aqueous solution, continue to stir for 3 hours to obtain a white turbid solution, age the white turbid solution at a constant temperature of 120°C for 2 hours, after the aging is completed, obtain a precipitated mixture, filter the precipitated mixture to obtain a white filter cake, and remove the white After the filter cake was washed with distilled water and absolute ethanol for 3 times in sequence, the filter cake was dried at 80°C for 24 hours to obtain a white product, that is, hollow microspheres of magnesium borate with a hierarchical structure. The magnesium borate has a microcrystalline structure as detected by XRD, and the composition is Mg 7 B 4 o 13 ·7H 2 O, its diffraction peak ...

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Abstract

The invention discloses a preparation method of multi-level structure magnesium borate hollow microspheres. The method comprises the following steps of: taking an inorganic magnesium salt water solution in the molar concentration of 0.01-0.20mol / L and a borax water solution in the molar concentration of 0.01-0.20mol / L as raw materials, stirring in ionic liquid at room temperature for 2-5 hours, aging for 2-72 hours at the temperature of 20-120 DEG C to get a precipitate mixture, filtering the precipitate mixture, washing a filter cake, drying and / or calcining at the temperature of 300-900 DEG C in an air atmosphere to get the multi-level structure magnesium borate hollow microspheres. The magnesium borate microspheres with better crystal form and hollow structure can be obtained by the preparation method disclosed by the invention, and the preparation method has the advantages of simple process, easiness in operation, high yield, complete crystal form of products, more uniform size distribution and high purity.

Description

(1) Technical field [0001] The invention relates to a preparation method of hollow microspheres, in particular to a preparation method of magnesium borate hollow microspheres with a hierarchical structure. (2) Background technology [0002] With the development of nanoscience and technology, nanostructures with special morphology have attracted more and more people's interest and attention. Due to its low density, high specific surface area, monodispersity and high stability, and its hollow part can accommodate other materials, the hollow inorganic micro / nanostructure can produce some peculiar properties based on the microscopic "wrapping" effect, making the hollow Micro / nanostructures have important applications in many technical fields such as microscale reactors, drug delivery carriers, photonic crystals, catalysts, and energy storage, and have become the frontier and hot spot in the field of nanomaterial science. At present, metals (Ni, Co, Cu, Pd, Pt, Ag, Au, etc.), ox...

Claims

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Application Information

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IPC IPC(8): C01B35/12B82Y40/00
Inventor 陈爱民顾培
Owner 海宁市黄湾镇资产经营有限公司
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