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Preparation method of polycrystalline mullite fiber

A polycrystalline mullite and fiber technology, applied in the direction of inorganic raw materials such as artificial filaments, can solve the problems of strict equipment requirements, difficult process control, high production costs, etc., and achieve tight bonding, uniform grain size, and complete crystal phase structure Effect

Inactive Publication Date: 2017-05-31
SHAANXI SHENGMAI PETROLEUM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process of using metal alkoxide as the main raw material has high production costs, strict requirements on equipment, difficult process control, and difficulty in achieving large-scale industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] With water as solvent, aluminum powder, AlCl 3 Reflux the raw material to obtain a colorless and transparent polyaluminum chloride sol; add acidic silica sol, add spinning aid, concentrate in vacuum, and remove part of the free water to obtain a viscous precursor sol; prepare the precursor by spinning the sol through the spinning method Fiber, the obtained precursor fiber is dried and heat-treated to finally produce polycrystalline mullite fiber.

[0019] Wherein, the reflux temperature is 90° C., and the reflux time is 5 hours. Said adding to the acidic silica sol, the amount of substance m (Al):m (Si)=3:1. The described spinning aid is 3% polyvinyl alcohol in mass fraction. The viscosity of the precursor sol is 4000. The drying temperature is 60° C., and the drying time is 4 hours. The heat treatment temperature is 800° C., and the heat treatment time is 2 hours. The temperature of the vacuum concentration is 50°C.

Embodiment 2

[0021] With water as solvent, aluminum powder, AlCl 3 Reflux the raw material to obtain a colorless and transparent polyaluminum chloride sol; add acidic silica sol, add spinning aid, concentrate in vacuum, and remove part of the free water to obtain a viscous precursor sol; prepare the precursor by spinning the sol through the spinning method Fiber, the obtained precursor fiber is dried and heat-treated to finally produce polycrystalline mullite fiber.

[0022] Wherein, the reflux temperature is 100° C., and the reflux time is 8 hours. Said adding to the acidic silica sol, the amount of substance m (Al):m (Si)=3:1. The described spinning aid is 3% polyvinyl alcohol in mass fraction. The viscosity of the precursor sol is 6000. The drying temperature is 80° C., and the drying time is 6 hours. The heat treatment temperature is 1300° C., and the heat treatment time is 3 hours. The temperature of the vacuum concentration is 60°C.

Embodiment 3

[0024] With water as solvent, aluminum powder, AlCl 3 Reflux the raw material to obtain a colorless and transparent polyaluminum chloride sol; add acidic silica sol, add spinning aid, concentrate in vacuum, and remove part of the free water to obtain a viscous precursor sol; prepare the precursor by spinning the sol through the spinning method Fiber, the obtained precursor fiber is dried and heat-treated to finally produce polycrystalline mullite fiber.

[0025] Wherein, the reflux temperature is 95°C, and the reflux time is 6h. Said adding to the acidic silica sol, the amount of substance m (Al):m (Si)=3:1. The described spinning aid is 3% polyvinyl alcohol in mass fraction. The viscosity of the precursor sol is 4000. The drying temperature is 70° C., and the drying time is 5 hours. The heat treatment temperature is 1000° C., and the heat treatment time is 2 hours. The temperature of the vacuum concentration is 55°C.

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Abstract

The invention relates to the technical field of functional materials and particularly relates to a preparation method of a polycrystalline mullite fiber. The preparation method of the polycrystalline mullite fiber comprises the following steps: carrying out reflux at 90-100 DEG C for 5-8 hours by taking water as a solvent as well as powdered aluminum and AlCl3 as raw materials, so as to obtain colorless transparent poly aluminium chloride sol; adding acidy silica sol according to a mount that m(Al):m(Si)=3:1, and carrying out vacuum concentration at 50-60 DEG C by taking 3% polyvinyl alcohol as a spinning aid so as to remove partial free water, so as to obtain precursor sol with a viscosity of 4000-6000; and preparing a precursor fiber from the precursor sol by virtue of a thread throwing method, drying the obtained precursor fiber at 60-80 DEG C for 4-6 hours, and carrying out thermal treatment at 800-1300 DEG C for 2 hours, so as to finally obtain the polycrystalline mullite fiber. The polycrystalline mullite fiber prepared by virtue of the preparation method has the beneficial effects that the crystal structure tends to be complete, the fiber diameter is 3-6 microns, and grains are uniform in size and tightly jointed.

Description

technical field [0001] The invention relates to the technical field of functional materials, in particular to a preparation method of polycrystalline mullite fibers. Background technique [0002] Polycrystalline mullite fiber is a high-performance inorganic fiber, which is composed of mullite microcrystals and has the characteristics of high temperature resistance, creep resistance, thermochemical stability, low thermal expansion coefficient, small thermal conductivity and high modulus. , Widely used in metallurgy, machinery, ceramics, electronics, building materials, petrochemical, aerospace and other fields. In addition, polycrystalline mullite fiber also has good infrared radiation, insulation, sound attenuation, anti-oxidation, and oil resistance. [0003] The sol-gel method is one of the main methods for preparing polycrystalline mullite fibers. At present, the main raw materials for preparing polycrystalline mullite fibers by sol-gel method are mostly expensive metal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F9/08D01F1/10
CPCD01F9/08D01F1/10
Inventor 王耀斌
Owner SHAANXI SHENGMAI PETROLEUM
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