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Preparing method for porous Fe-Si-C ceramic micro balls

A technology of ceramic microspheres and fe-si-c, which is applied in the field of preparation of porous Fe-Si-C ceramic microspheres obtained by cracking, can solve the problem that Fe-Si-C ceramic microspheres have not been reported and the preparation of SiC ceramic microspheres The method is limited and other problems, to achieve the effect of being suitable for large-scale production, narrow particle size distribution, and good stability

Active Publication Date: 2015-06-10
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, the current preparation methods of SiC ceramic microspheres are very limited, and the preparation of Fe-Si-C ceramic microspheres has not been reported.

Method used

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  • Preparing method for porous Fe-Si-C ceramic micro balls
  • Preparing method for porous Fe-Si-C ceramic micro balls
  • Preparing method for porous Fe-Si-C ceramic micro balls

Examples

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reference example 1

[0036] Reference example 1: the preparation of ferrocene lithium salt:

[0037]Vacuumize the synthesis reaction system, replace high-purity nitrogen to normal pressure, repeat 3 times; add 10 g (53.8 mmol) ferrocene and 70 mL of anhydrous n-hexane solvent into a dry 250 mL reaction bottle, stir; then add 10 mL (66.7 mmol) of tetramethylethylenediamine; after stirring evenly, add 53 mL of n-hexane solution with a molar concentration of n-butyllithium of 2.4 mol / L dropwise, stir, and react for 10 h; filter under reduced pressure, remove the filtrate, Adopt anhydrous n-hexane to wash the orange-red solid filter residue 3 times, and vacuum-dry to remove the n-hexane in the filter residue to obtain 13.3 g ferrocene lithium salt (Fe(η-C 5 h 4 Li 2 )·2 / 3TMEDA). The dried lithium ferrocene salt was stored in an argon-protected glove box.

reference example 2

[0038] Reference example 2: Synthesis of polyferrocenyl silane:

[0039] Vacuumize the synthesis reaction system, replace high-purity nitrogen to normal pressure, repeat 3 times, take 5 g (18.2 mmol) of ferrocene lithium salt prepared in Reference Example 1 in a 250 mL reaction bottle in the glove box, seal it well Remove and place in a -20°C reaction bath, inject 50 mL of anhydrous tetrahydrofuran (THF) with a syringe, stir to dissolve; then add Cl dropwise through a constant pressure dropping funnel 2 Si(CH 3 ) 2 solution in THF (0.94 g (7.3 mmol) Cl 2 Si(CH 3 ) 2 Dissolved in 30 mL THF), stirred at -20°C for 1 h; then added Cl dropwise through a constant pressure dropping funnel 3 SiCH 3 solution in THF (1.09 g (7.3 mmol) Cl 3 Si CH 3 dissolved in 30 mL THF), stirred at 25°C for 12 hours; finally, 1 mL of methanol was added dropwise to terminate the reaction, filtered, the filtrate was concentrated to 20 mL, the concentrated solution was added dropwise to the stir...

Embodiment 1

[0041] (1) Dissolve 0.3 g PFS in 2.7 mL of an organic solvent (a solvent mixed with tetrahydrofuran and xylene at a volume ratio of 2:1), stir, and prepare a 3 mL polymer solution with a mass fraction of 10 wt %, and stir to obtain a composite Part a; (2) Dissolve 20 g of gelatin in 180 mL of deionized water at 80°C, stir to form 200 mL of gelatin emulsion with a mass fraction of 10wt%, and obtain component b; (3) At 60°C, stir at a speed of 300 At r / min, drop the component a obtained in step (1) into the component b obtained in step (2) with a rubber dropper, micro-droplets appear, continue to stir for 4 h, let stand, and the polymer microspheres sink in At the bottom, pour the upper emulsion, add 1L of deionized water, dilute the gelatin emulsion containing polymer microspheres, filter, collect the microspheres, then wash the microspheres with deionized water for 3 times, wash with ethanol for 2 times, and finally at 55 °C, Vacuum-dried for 8 h to obtain polymer microspheres...

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Abstract

A preparing method for porous Fe-Si-C ceramic micro balls comprises the following steps that firstly, poly-ferrocenylsilanes is dissolved in an organic solvent and stirred, deionized water and a surface active agent are added or not added, stirring is carried out, and a component a is obtained; secondly, gelatin or polyving akohol are dissolved in the deionized water, stirring is carried out, and a component b is obtained; thirdly, the component a is dripped in the component b to continue to be stirred, the mixture stands still, the upper layer emulsion is poured, the deionized water is added for dilution, filtering is carried out, micro balls are collected and cleaned, finally, vacuum drying is carried out, and polymeric micro balls are obtained; fourthly, the polymeric micro balls obtained in the third step are sintered and split in a tubular stove, and the porous Fe-Si-C ceramic micro balls are obtained. The preparing method is simple and convenient to implement, the shape of the obtained porous Fe-Si-C ceramic micro balls is regular, a multi-level pore structure is arranged inside, a large number of nanometer Fe particles with the catalysis function are evenly distributed, and the porous Fe-Si-C ceramic micro balls have very good application prospects in the catalyst carrier field.

Description

technical field [0001] The invention relates to a method for preparing porous Fe-Si-C ceramic microspheres, in particular to a method for preparing porous Fe-Si-C ceramic microspheres by cracking polyferrocenyl silane as a precursor. Background technique [0002] Ceramic microspheres generally refer to inorganic non-metallic polycrystalline spheres with a particle size of micron, which are available in the form of solid, hollow and porous microspheres, and are widely used in military, pharmaceutical, chemical, nuclear technology and other industries. Among them, porous ceramic microspheres are mostly used as separation and purification media due to their high strength, stable chemical properties, and regular and uniform pore structure; due to their large specific surface area and roughness, the loaded substances are relatively easy and permanent immobilization, so they are often used as catalysts and drug carriers. [0003] At present, the preparation methods of ceramic mic...

Claims

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Application Information

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IPC IPC(8): C04B35/56C04B35/626
Inventor 苟燕子王浩童旋毛腾飞
Owner NAT UNIV OF DEFENSE TECH
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