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A kind of preparation method of porous fe-si-c ceramic microsphere

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 pyrolysis, can solve the problem of limited preparation methods of SiC ceramic microspheres and the unresolved problems of Fe-Si-C ceramic microspheres. See reports and other issues, and achieve the effect of being suitable for large-scale production, easy to operate, and good stability

Active Publication Date: 2016-09-14
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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  • A kind of preparation method of porous fe-si-c ceramic microsphere
  • A kind of preparation method of porous fe-si-c ceramic microsphere
  • A kind of preparation method of porous fe-si-c ceramic microsphere

Examples

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Effect test

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 polyferrocenylsilane:

[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 s...

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 preparation method of porous Fe-Si-C ceramic microspheres, comprising the following steps: (1) dissolving polyferrocene-based silane in an organic solvent, stirring, adding or not adding deionized water and a surfactant, stirring, Obtain component a; (2) Dissolve gelatin or polyvinyl alcohol in deionized water and stir to obtain component b; (3) drop component a into component b, continue to stir, let it stand, and pour the upper emulsion , add deionized water to dilute, filter, collect the microspheres, then wash the microspheres, and finally dry them in vacuum to obtain polymer microspheres; (4) Burn and crack the polymer microspheres obtained in step (3) in a tube furnace , Porous Fe‑Si‑C ceramic microspheres. The preparation method of the invention is simple and convenient, and the obtained porous Fe-Si-C ceramic microspheres have a regular shape, have a multi-level pore structure inside, and are evenly distributed with a large number of nano-Fe particles with catalytic functions, and have good application prospects in the field of catalyst carriers.

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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Patent Type & Authority Patents(China)
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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