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A kind of precursor sol for continuous alumina fiber and its application

A technology of alumina fiber and precursor solution, which is applied in the fields of fiber chemical characteristics, textiles and papermaking, etc., can solve the problems of being unsuitable for large-scale industrial production and toxicity, and achieves easy large-scale industrial production, stable properties, and reduced precipitation The effect produced

Active Publication Date: 2021-11-16
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, the patent [see US Patent 495462] reports a method for preparing continuous alumina fibers. Aluminum carboxylate sol is prepared by using aluminum powder, formic acid, and acetic acid system. At the same time, catalysts such as aluminum nitrate need to be added. The whole reaction conditions are relatively harsh. It can be prepared when boiling; literature [referring to: Journal of Silicates, 1997, 25 (3): 339-344.] reports that mercuric chloride is used as a catalyst to prepare aluminum carboxylate system precursor sol, because mercuric chloride is toxic, Not suitable for large-scale industrial production

Method used

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  • A kind of precursor sol for continuous alumina fiber and its application
  • A kind of precursor sol for continuous alumina fiber and its application
  • A kind of precursor sol for continuous alumina fiber and its application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] A kind of precursor sol for continuous alumina fiber, its preparation method, comprises steps as follows:

[0050] (1) Add 250g of deionized water to a 1L three-necked round-bottomed flask, add 16g of formic acid and 18g of acetic acid under the condition of reflux at 90°C, stir for 15min, and add a total of 13.5g of aluminum powder (particle size 20μm) in 5 times at intervals of 30min ). After continuing the reaction and stirring for 1 hour, add 28.35 g of nitric acid with a mass fraction of 40% dropwise. After the total reaction time reaches 18 hours, the reaction is stopped, and the aluminum powder is completely dissolved. After the reaction solution is cooled, filter impurities with filter paper to obtain a clear and transparent alumina precursor. body sol.

[0051] (2) 10 g of polyvinylpyrrolidone with an average molecular weight of 130,000 was dissolved in 90 g of deionized water to prepare a 10% spinning aid solution.

[0052] (3) Add 30 g of the spinning aid p...

Embodiment 2

[0061] A kind of precursor sol for continuous alumina fiber, its preparation method, comprises steps as follows:

[0062] (1) Add 250g of deionized water to a 1L three-neck round-bottom flask, add 8g of formic acid, 9g of acetic acid, 2g of citric acid, and 3g of oxalic acid under reflux at 85°C. After stirring for 15 minutes, add a total of 13.5g in 3 times at intervals of 30 minutes each time Aluminum powder (particle size 20μm). After continuing to react and stir for 1.5h, add 56g of nitric acid with a mass fraction of 45% dropwise. After the total reaction time reaches 30h, the reaction is stopped, and the aluminum powder is completely dissolved. After the reaction solution is cooled, filter impurities with filter paper to obtain a clear and transparent alumina precursor. body sol.

[0063] (2) 5 g of polyvinylpyrrolidone with an average molecular weight of 580,000 was dissolved in 90 g of deionized water to prepare a 5% spinning aid solution.

[0064] (3) Add 20 g of th...

Embodiment 3

[0069] A kind of precursor sol for continuous alumina fiber, its preparation method, comprises steps as follows:

[0070] (1) Add 300g of deionized water to a 1L three-neck round-bottomed flask, add 6.9g of formic acid and 7.5g of acetic acid under reflux conditions at 100°C, and stir for 10 minutes, add a total of 13.5g of aluminum flakes (thickness 1mm, length 10cm, width 2cm). After continuing the reaction and stirring for 1 hour, add 12 g of nitric acid with a mass fraction of 40% dropwise. After the total reaction time reaches 24 hours, the reaction is stopped, and the aluminum flakes are completely dissolved. After the reaction solution is cooled, filter impurities with filter paper to obtain a clear and transparent alumina precursor Sol.

[0071] (2) Dissolve 15 g of polyvinyl alcohol with an average degree of polymerization of 1788 and a degree of alcoholysis of 99% in 90 g of deionized water to prepare a 15% spinning aid solution.

[0072] (3) Add 15 g of the spinni...

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Abstract

The invention relates to a spinnable alumina precursor sol and application thereof. The sol is prepared by the following scheme: select elemental aluminum, divide the elemental aluminum into N parts; mix the organic acid and water evenly, and then add the first part of elemental aluminum; condense and reflux under the condition of 100 ° C or less; During the reflux process, add the remaining elemental aluminum to the system at least twice to continue condensing and refluxing. After the elemental aluminum is completely added, continue to reflux for at least 1 hour; then add the catalyst; continue to condense and reflux for at least 1 hour; cool, filter, and obtain continuous oxidation Precursor sol for aluminum fiber preparation. The preparation process of the present invention is simple, pollution-free, green and circular, and easy for large-scale industrial production and preparation. The sol can be dry-spun and calcined to prepare continuous alumina fibers and alumina-based ceramic fibers. The products can be used in thermal insulation, military and national defense, aerospace, chemical and environmental protection and other fields.

Description

technical field [0001] The invention relates to a precursor sol for continuous alumina fibers and an application thereof. The sol can be used in the preparation of continuous alumina fibers and alumina-based ceramic fibers, and belongs to the field of inorganic ceramic materials. Background technique [0002] Alumina fiber, also known as polycrystalline alumina fiber, belongs to high-performance inorganic fiber. It is a kind of polycrystalline ceramic fiber, which has various forms such as long fiber, short fiber and whisker. 2 o 3 as the main component, and contains a small amount of SiO 2 , B 2 o 3 , MgO and other additives. Continuous alumina fibers have the advantages of high strength, extraordinary heat resistance and high temperature oxidation resistance, and can maintain good tensile strength at higher temperatures. Continuous alumina fiber has good surface activity and is easy to compound with resin, metal and ceramic matrix to form many composite materials with...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F9/10
CPCD01F9/10
Inventor 马运柱刘强王娟刘文胜姚树伟程铭刘继进
Owner CENT SOUTH UNIV
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