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A kind of melt-spinning raw material of alumina continuous fiber, its preparation method and prepared alumina continuous fiber

A technology of melt spinning and continuous fiber, which is applied in the fields of fiber chemical characteristics, rayon manufacturing, textiles and paper making, etc. It can solve problems such as low melt viscosity, high melting point of alumina ceramics, and difficulty in preparing alumina precursors. Achieve the effect of simple equipment requirements, stable quality, and large-scale industrial production

Active Publication Date: 2019-08-20
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the strong metallicity of Al atoms, it is difficult to prepare alumina precursors that can be melted, so there is no report on the preparation of alumina fibers by melt spinning of precursors, and alumina ceramics have a high melting point and the viscosity of the melt Low, so it cannot be produced by traditional fusion drawing method like quartz fiber

Method used

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  • A kind of melt-spinning raw material of alumina continuous fiber, its preparation method and prepared alumina continuous fiber
  • A kind of melt-spinning raw material of alumina continuous fiber, its preparation method and prepared alumina continuous fiber
  • A kind of melt-spinning raw material of alumina continuous fiber, its preparation method and prepared alumina continuous fiber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Preparation of alumina fiber by direct melt spinning of PAO-P without adding powder

[0053] 1. Preparation of melt spinning raw materials:

[0054] Preparation of melt-spinning alumina precursor: put 500g of polyaluminoxane in a reaction kettle, heat to 80°C under stirring, distill under reduced pressure for 1h, continue to heat up to 120°C, keep warm for 1h, and finally raise the temperature to 160°C , take a sample every 10 minutes to measure the softening point, when the softening point reaches 90 ° C, stop heating, nitrogen protection down to room temperature to obtain the polymerized alumina precursor PAO-P;

[0055] 2. Preparation of alumina fibers

[0056] (1) Melt spinning: put the spinning raw material in the spinning cylinder of the melt spinning device, heat it up to 150°C under the protection of nitrogen, and wait for it to melt into a uniform melt and remove residual bubbles, then carry out at 120°C Melt spinning, bundled and collected to obtain continuo...

Embodiment 2

[0062] Preparation of alumina fiber by direct melt spinning of PAO-P without adding powder

[0063] 1. Preparation of melt spinning raw materials:

[0064] Preparation of melt-spinning alumina precursor: put 500g of polyaluminoxane in a reaction kettle, heat to 85°C under stirring, distill under reduced pressure for 2h, continue to heat up to 140°C, keep warm for 1h, and finally raise the temperature to 170°C , take a sample every 10 minutes to measure the softening point, when the softening point reaches 120 ° C, stop heating, nitrogen protection down to room temperature to obtain the polymerized alumina precursor PAO-P;

[0065] 2. Preparation of alumina fibers

[0066] (1) Melt spinning: put the spinning raw material in the spinning cylinder of the melt spinning device, heat it up to 180°C under the protection of nitrogen, and wait for it to melt into a uniform melt and remove residual bubbles, then carry out at 150°C Melt spinning, bundled and collected to obtain continu...

Embodiment 3

[0072] 1. Preparation of melt spinning raw materials:

[0073] (1) Preparation of melt-spinning alumina precursor: put 500g of polyaluminoxane in a reaction kettle, heat it to 80°C under stirring, distill under reduced pressure for 1h, continue to heat up to 120°C, keep it warm for 1h, and finally raise the temperature again To 180°C, take samples every 10 minutes to measure the softening point, when the softening point reaches 113°C, stop heating, nitrogen protection down to room temperature to obtain polymerized alumina precursor PAO-P;

[0074] (2) Preparation of powder slurry: polyaluminoxane (PAO) and polyethylene glycol (PEG-200) were refluxed in n-propanol for 1 h, polyaluminoxane (PAO), polyethylene glycol ( The mass ratio of PEG-200) and n-propanol is 1:0.2:1, and decompression solvent removal obtains dispersant (PAO-S); Dispersant, particle diameter are the α-Al of 150nm 2 o 3 Put the powder and n-propanol in a sand mill at a mass ratio of 1:1.5:3 and grind at a fr...

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Abstract

The invention relates to a melt spinning raw material for alumina continuous fiber, and a preparation method thereof, and alumina continuous fiber prepared from the melt spinning raw material. The preparation method comprises: 1) placing polyaluminoxane in a reaction kettle, heating to a temperature of 60-100 DEG C, carrying out pressure reducing distillation, continuously heating to a temperatureof 110-140 DEG C, carrying out thermal insulation, heating to a temperature of 150-200 DEG C, sampling, determining softening points, stopping the heating after the determined softening point achieves a target softening point, and cooling to a room temperature to obtain a solid alumina precursor PAO-P; 2) mixing a dispersant, aluminum-containing powder and a solvent according to a mass ratio of 1:(1.5-4):(3-6), and grinding to obtain a powder slurry; and 3) mixing the obtained precursor and the obtained powder slurry, heating to a temperature of 150-200 DEG C, and carrying out pressure reducing distillation to obtain the melt spinning raw material. According to the present invention, with the method, the alumina precursor PAO-P capable of being subjected to melt spinning is synthesized, the melt spinning and sintering process of the alumina fiber precursor is provided, and the defect that the alumina continuous fiber cannot be prepared through the melt spinning is overcome.

Description

technical field [0001] The invention belongs to the field of preparation of ceramic fibers, in particular, relates to the preparation of inorganic oxide ceramic fibers, in particular to a melt spinning raw material of alumina continuous fibers, its preparation method and the prepared alumina continuous fibers. Background technique [0002] Alumina fiber is a high-performance inorganic fiber. It starts with Al 2 o 3 As the main component, some also contain other metal oxides such as ZrO 2 and SiO 2 Etc., with long fiber, short fiber, whisker and other forms. The outstanding advantages of alumina fiber are high strength, high modulus, and excellent mechanical properties in an air atmosphere of 1000-1200 ° C. At the same time, it also has the advantages of small thermal conductivity, low thermal expansion coefficient, and good thermal shock resistance. In addition, compared with other high-performance inorganic fibers such as silicon carbide fibers, the raw material cost o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F9/10D01F1/10C04B35/10C04B35/622
Inventor 赵彤李敬毓韩伟健叶丽
Owner INST OF CHEM CHINESE ACAD OF SCI
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