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A kind of method that titanium-aluminum polymer precursor prepares aluminum titanate ceramic fiber

A ceramic fiber and polymer technology, applied in the chemical characteristics of fibers, textiles and papermaking, etc., can solve the problems of poor fiber performance, high energy consumption of solid-phase method, high fiber porosity, and achieve good thermal shock resistance and easy batch production. The effect of chemical production and low thermal expansion coefficient

Active Publication Date: 2022-04-29
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Aluminum titanate fibers made of aluminum titanate can be used as fire-resistant and heat-insulating materials, and have broad application prospects in many fields. However, there are certain defects in the literature reports on aluminum titanate fibers. For example, Chinese patent document 200710166722.4 discloses a A method for preparing aluminum titanate fiber spinnable sol, but the sol preparation process involved in the invention involves acid corrosion and vacuum treatment, which requires high equipment and high preparation costs, and if it is necessary to prepare aluminum titanate nanofibers, it is necessary to Need to further improve the spinnability of the sol
[0005] Chinese patent document 20101013320.X discloses an aluminum titanate nanofiber and its preparation method. The invention uses a hydrothermal method, and its hydrothermal reaction temperature is difficult to control, which is technically difficult and has poor safety performance.
These preparation methods all have certain defects. The melting method is difficult to control chemical composition, purity, crystallite distribution and particle size, etc., and the synthesis temperature is high, which is not suitable for synthesizing ceramic fibers with high melting point; the impregnation method has a long production cycle and large energy consumption. Fiber breakage and pulverization are easy to occur when the template is removed, the fiber uniformity is poor, and the performance is unstable; the chemical vapor deposition method requires expensive special equipment and high control requirements; the fiber obtained by the ultrafine powder extrusion spinning method has high porosity and crystal The particle size is large, the strength is low, and the fiber performance is poor; the solid-phase method has defects such as high energy consumption and uneven particles; although the sol-gel method is uniform and stable due to the prepared sol, it has good spinnability, adjustable components, and high sample purity. , but the reaction conditions are difficult to control, the diameter of the fiber prepared by the sol obtained by the sol-gel method is relatively large, the requirements for the spinnability of the precursor sol are relatively high, and the sol spinning solution is unstable, etc.

Method used

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  • A kind of method that titanium-aluminum polymer precursor prepares aluminum titanate ceramic fiber
  • A kind of method that titanium-aluminum polymer precursor prepares aluminum titanate ceramic fiber
  • A kind of method that titanium-aluminum polymer precursor prepares aluminum titanate ceramic fiber

Examples

Experimental program
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Effect test

Embodiment 1

[0051] A method for preparing aluminum titanate fibers using titanium-aluminum polymer as a precursor, comprising the following preparation steps:

[0052] (1) According to the molar ratio of titanium tetrachloride: anhydrous aluminum chloride: distilled water: acetylacetone: triethylamine=1:2:3:3:10, take by weighing 20g titanium tetrachloride, 28g anhydrous chlorine Aluminum chloride, 5.7g distilled water, 32g acetylacetone and 106g triethylamine, and respectively diluted in 40g, 140g, 2.85g with 1:2, 1:5, 1:0.5, 1:1 and 1:1 and mass ratio , 32g and 106g in five parts of anhydrous methanol, under ice bath conditions, add anhydrous aluminum chloride methanol solution to the stirring titanium tetrachloride methanol solution, continue stirring for 30min after adding and keep the ice bath, Obtain solution A, then add distilled water, acetylacetone and triethylamine methanol solution dropwise to the mixed solution A, and continue to stir under ice bath for 12 hours to fully react...

Embodiment 2

[0058] As described in Example 1, the method for preparing aluminum titanate fibers using titanium-aluminum polymer as a precursor, the difference is that

[0059] In step (1), the methanol solution of anhydrous aluminum chloride is added to the methanol solution of titanium tetrachloride instead of the methanol solution of titanium tetrachloride added to the methanol solution of anhydrous aluminum chloride, and the obtained fiber is the same as that of Example 1 The fibers obtained were virtually indistinguishable.

Embodiment 3

[0061] As described in Example 1, the method for preparing aluminum titanate fibers using titanium-aluminum polymer as a precursor, the difference is that

[0062] In step (2), change the mass ratio of titanium-aluminum polymer precursor: anhydrous methanol: PEO to 100:100:1, that is, dissolve 5g titanium-aluminum polymer precursor and 0.05g PEO in 5g anhydrous methanol Among them, the obtained fiber diameter is larger, the fiber diameter is about 1 μm, and the yield is improved.

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Abstract

The invention relates to a method for preparing aluminum titanate ceramic fibers from a titanium-aluminum polymer precursor. The method is to obtain the titanium-aluminum polymer precursor on the basis of metal coordination chemistry, add spinning aids to the titanium-aluminum polymer precursor sol, and obtain the sol-spinning solution. Under high temperature conditions, the solvent volatilizes, and the solute solidifies into titanium-aluminum polymer precursor fibers. The prepared aluminum titanate ceramic fibers not only have good high temperature resistance, but also maintain good fiber morphology under high temperature conditions up to 1400 ° C, and have Low thermal expansion coefficient and good thermal shock resistance.

Description

technical field [0001] The invention relates to a method for preparing aluminum titanate ceramic fibers from a titanium-aluminum polymer precursor, and belongs to the field of inorganic refractory ceramic fiber materials. Background technique [0002] With the rapid development of modern industry and high-temperature technology, the demand for fiber materials with comprehensive properties such as high temperature resistance and thermal shock resistance is becoming more and more urgent. Traditional materials such as aluminum silicate can no longer meet the high temperature requirements above 1350 °C requirements of harsh environments. Aluminum titanate (Al 2 TiO 5 ) not only has a high melting point (1860±10℃), low thermal expansion coefficient (α<1.5×10 -6 / °C), low thermal conductivity (1.5W / (m K)), etc., also has good thermal shock resistance, strong acid and alkali corrosion resistance, good thermal shock resistance, and no infiltration of metal and glass melts, etc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/478C04B35/622C08G79/10D01F9/10
CPCC04B35/478C04B35/62231C04B35/62236C04B35/62259D01F9/10C08G79/10C04B2235/96C04B2235/9607
Inventor 朱陆益刘伟谢永帅许东王新强张光辉
Owner SHANDONG UNIV
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