Method for preparing mullite nanofibers by combination of non-hydrolytic sol-gel technology and electrostatic spinning technology

A nanofiber, electrospinning technology, used in fiber processing, textile and papermaking, filament/thread forming, etc., can solve the problems of clogging the nozzle, difficult to obtain uniform size fibers continuously, temperature dependence, etc.

Inactive Publication Date: 2013-07-31
NORTH CHINA UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the metal alkoxide hydrolyzed sol is an unstable system that is dependent on temperature. During the electrospinning process, it is often accompanied by reaction processes such as hydrolysis, coagulation, and gelation. The viscosity of the system also changes with time, resulting in frequent coarse Fiber formation, in severe cases, will block the nozzle, making it difficult to continuously obtain fibers of uniform size
For this reason, it is necessary to add a catalyst to the solution to adjust the rate of hydrolysis and gelation, and to reduce the rate of hydrolysis and gelation by reducing the ambient humidity near the jet or saturating the solvent around it, resulting in complicated spinning operations. Increased preparation costs

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Using 6.12g of anhydrous aluminum trichloride and 3.99ml of tetraethyl orthosilicate as the precursor, 6.27ml of isopropyl ether as the oxygen donor, and 30ml of anhydrous dichloromethane as the solvent, put the reaction solution into the reaction bomb Put it in an oven at 110°C for 13h to synthesize the precursor gel, and then dry the gel at 70°C for 3h to obtain the mullite xerogel. Measure absolute ethanol and tetrahydrofuran at 70% and 30% by mass and mix them to obtain a mixed solution A. Dissolve the above-mentioned mullite xerogel with a mass percentage of 2% in the mixed solution A with a mass percentage of 98%. Obtain mixed solution B; mix and stir polyvinylpyrrolidone (PVP, molecular weight: 1,300,000) with mixed solution B at 5% and 91% by mass, and then add dropwise 4% N-N dimethylformamide to prepare Spinning precursor solution. According to the spinning parameters, the spinning voltage is 15KV, the feeding speed is 0.6ml / h, and the solidification distance...

Embodiment 2

[0015] Using 6.12g of anhydrous aluminum trichloride and 3.99ml of tetraethyl orthosilicate as the precursor, 6.27ml of isopropyl ether as the oxygen donor, and 30ml of anhydrous dichloromethane as the solvent, put the reaction solution into the reaction bomb Put it in an oven at 120°C for 12h to synthesize the precursor gel, and then dry the gel at 60°C for 4h to obtain the mullite xerogel. Measure absolute ethanol and tetrahydrofuran at 70% and 30% by mass and mix them to obtain a mixed solution A. Dissolve the above-mentioned mullite xerogel with a mass percentage of 2% in the mixed solution A with a mass percentage of 98%. Obtain mixed solution B; be 5% and 90% by mass percentage polyvinylpyrrolidone (PVP, molecular weight is 58000) mix with mixed solution B, then add dropwise the N-N dimethyl formamide that is 5% by mass percentage, prepare spinning precursor. According to the spinning parameters, the spinning voltage is 15KV, the feeding speed is 0.6ml / h, and the solidi...

Embodiment 3

[0017]Using 7.34 ml of anhydrous aluminum trichloride and 4.79 ml of tetraethyl orthosilicate as the precursor, 7.52 ml of isopropyl ether as the oxygen donor, and 36 ml of anhydrous dichloromethane as the solvent, put the reaction solution into the reaction bomb. Put it in an oven at 130°C for 10h to synthesize the precursor gel, and then dry the gel at 50°C for 5h to obtain the mullite xerogel. Measure absolute ethanol and THF at 65% and 35% by mass and mix them to obtain a mixed solution A. Dissolve the above-mentioned mullite xerogel with a mass percentage of 1.5% in mixed solution A with a mass percentage of 98.5%. Obtain mixed solution B; be 13% and 84% by mass percentage polyvinylpyrrolidone (PVP, molecular weight is 1000000) and mix solution B, then add dropwise the N-N dimethylformamide that mass percentage is 3%, prepare spinning precursor. According to the spinning parameters, the spinning voltage is 15KV, the feeding speed is 0.6ml / h, and the solidification distan...

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Abstract

The invention relates to a method for preparing mullite nanofibers by combination of a non-hydrolytic sol-gel technology and an electrostatic spinning technology, and belongs to the technical field of material science. The method comprises that anhydrous aluminum chloride and tetraethoxysilane as raw materials, isopropyl ether as an oxygen donor and anhydrous dichloromethane as a solvent are synthesized into mullite xerogel by the non-hydrolytic sol-gel method; anhydrous ethanol and tetrahydrofuran are mixed into a mixed solution A; the mullite xerogel is dissolved in the mixed solution A so that a mixed solution B is obtained; polyvinylpyrrolidone (PVP) and the mixed solution B are mixed by stirring; a less amount of N-N-dimethylformamide is dropwisely added into the mixture obtained by the previous step so that a spinning precursor is obtained; the spinning precursor is prepared into mullite xerogel/PVP composite fibers by an electrostatic spinning technology; and the mullite xerogel/PVP composite fibers are calcined at a temperature of 900 to 1200 DEG C and then are subjected to heat preservation for 0.5 to 5h to form the mullite nanofibers. The method has the advantages of simple processes, easy control and low preparation cost.

Description

technical field [0001] The invention belongs to the field of preparation of mullite fibers, in particular to a method for preparing mullite nanofibers by a non-hydrolytic sol-gel method combined with electrospinning. Background technique [0002] The chemical composition of mullite fiber is generally 3Al 2 o 3 2SiO2 2 , whose crystal phase is mullite, with [AlO 6 ] octahedral connection [AlO 4 ] tetrahedron and [SiO 4 ] Tetrahedral double chain formed by the stable framework, usually polycrystalline structure. It has good heat resistance, creep resistance, thermal shock resistance, good chemical stability and high temperature strength. The use temperature of mullite fiber is as high as 1500 ℃, and the tensile strength is about 2.1GPa. Therefore, it can be widely used in metallurgy, machinery, ceramics, electronics and aerospace and other fields. Mullite fiber is used in the roof lining of high-temperature kilns, which can reduce the weight of the kiln roof and improve...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F9/08D01D5/00
Inventor 魏恒勇魏颖娜姚少巍于守武王合洋乜海鹏卜景龙王瑞生王志发王榕林
Owner NORTH CHINA UNIVERSITY OF SCIENCE AND TECHNOLOGY
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