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Precursor sol for continuous alumina fibers and application thereof

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 toxicity and unsuitability for large-scale industrial production, and achieve stable properties, easy large-scale industrial production, and simple process Effect

Active Publication Date: 2021-01-08
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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 the solution is boiling; literature [refer 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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  • Precursor sol for continuous alumina fibers and application thereof
  • Precursor sol for continuous alumina fibers and application thereof
  • Precursor sol for continuous alumina fibers and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] A kind of precursor sol for continuous alumina fiber, its preparation method, comprises steps as follows:

[0049] (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, and stir for 15 minutes, then add a total of 13.5g of aluminum powder (particle size 20μm ). 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.

[0050] (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.

[0051] (3) Add 30 g of the spinning aid prepared in step (2) to t...

Embodiment 2

[0060] A kind of precursor sol for continuous alumina fiber, its preparation method, comprises steps as follows:

[0061] (1) Add 250g of deionized water to a 1L three-necked round-bottom flask, add 8g of formic acid, 9g of acetic acid, 2g of citric acid, and 3g of oxalic acid under the condition of 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.

[0062] (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.

[0063] ...

Embodiment 3

[0068] A kind of precursor sol for continuous alumina fiber, its preparation method, comprises steps as follows:

[0069] (1) Add 300g of deionized water to a 1L three-necked 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, then 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 the impurities with filter paper to obtain a clear and transparent alumina precursor Sol.

[0070] (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.

[0071] (3) Add 15 g of ...

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Abstract

The invention relates to spinnable alumina precursor sol and application thereof. According to the scheme, the sol is prepared by selecting simple substance aluminum, and dividing the simple substancealuminum into N parts; uniformly mixing organic acid with water, and then adding the first part of elemental aluminum; carrying out condensation reflux under the condition that the temperature is less than or equal to 100 DEG C; in the condensation reflux process, adding the residual simple substance aluminum into the system in at least two times to continue condensation reflux, and continuing reflux for at least one hour after the simple substance aluminum is completely added; then adding a catalyst; continuously condensing and refluxing for at least one hour; and cooling and filtering to obtain the precursor sol for preparing the continuous alumina fiber.s The method is simple in preparation process, free of pollution, environmentally friendly and capable of achieving large-scale industrial production and preparation easily. The sol can be used for preparing continuous alumina fibers and alumina-based ceramic fibers through dry spinning and calcining treatment, and the product can be applied to the fields of thermal insulation, military national defense, aerospace, chemical environmental protection and the like.

Description

technical field [0001] The invention relates to a precursor sol for continuous alumina fibers and its application. The sol can be used for 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 and 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 excell...

Claims

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Application Information

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Patent Type & Authority Applications(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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