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Method for preparing polyvinyl acetate zirconyl precursor sol spinning solution and sub-micron zirconium oxide crystal fibers

A technology of sol spinning solution and precursor fiber, which is applied in fiber processing, textiles and papermaking, filament/thread forming, etc., can solve the problems of low solid content of precursor spinning solution, insufficient diameter of zirconia crystal fiber, and It is difficult to guarantee the spinnability and fiber crystal quality at the same time, so as to achieve the effect of improving ultra-high temperature thermal insulation and mechanical properties, excellent ultra-high temperature thermal insulation and mechanical properties, and excellent thermal insulation and mechanical properties

Inactive Publication Date: 2017-07-07
山东德艾普节能材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In addition to the above-mentioned deficiencies in the prior art, the diameter of the zirconia crystal fiber is not fine enough, and there is no report on nanoscale or submicron high-quality zirconia crystal ultrafine fiber, the reason is that the solidity of the existing precursor spinning solution The content is low, and it is difficult to guarantee the spinnability and fiber crystal quality at the same time

Method used

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  • Method for preparing polyvinyl acetate zirconyl precursor sol spinning solution and sub-micron zirconium oxide crystal fibers
  • Method for preparing polyvinyl acetate zirconyl precursor sol spinning solution and sub-micron zirconium oxide crystal fibers
  • Method for preparing polyvinyl acetate zirconyl precursor sol spinning solution and sub-micron zirconium oxide crystal fibers

Examples

Experimental program
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Effect test

Embodiment 1

[0036] (1) Preparation of polyzirconyl acetate precursor sol spinning solution:

[0037] Weigh 300g of polyzirconyl acetate, 150g of glacial acetic acid, 45g of yttrium nitrate hexahydrate, and 5g of polyvinylpyrrolidone and dissolve them in 600g of anhydrous methanol under stirring. After the solid was completely dissolved and the reaction solution turned into a transparent solution, it was concentrated under reduced pressure at 35° C. until a colorless and transparent polyzirconyl acetate sol spinning solution with a density of 1.2 g / ml (measured at 25° C.) was obtained.

[0038] (2) Electrospinning

[0039] Add the polyzirconyl acetate sol spinning solution into a glass syringe with a 6# stainless steel needle, propel the spinning solution to flow out slowly by gravity, and cover the negative electrode receiving screen with aluminum foil to collect fibers. At a temperature of 25° C., a humidity of 45%, a voltage of 27 kV, and a receiving distance of 30 cm, the spinning sol...

Embodiment 2

[0045] As described in Example 1, the difference is that step (1) is concentrated under reduced pressure until obtaining a colorless and transparent polyzirconyl acetate spinning solution with a density of 1.08g / ml; in step (2), the stainless steel needle Change to 5#, change the humidity to 60%, and adjust the voltage to 36kV. The diameter of the obtained submicron zirconia crystal fiber is 500nm~1μm, the average diameter is 766nm, and the length is 1~25cm (such as image 3 shown), the contact between grains is close, and the orientation of adjacent grains is relatively consistent (such as Figure 4 shown).

Embodiment 3

[0047] As described in Example 1, the difference is that step (1) concentrates under reduced pressure until obtaining a colorless and transparent polyzirconyl acetate spinning solution with a density of 1.0 g / ml; in step (2), the stainless steel needle Change to 5#, change the humidity to 70%, adjust the voltage to 48kV, and the receiving distance is 25cm. The diameter of the obtained submicron zirconia crystal fiber is 100nm~400nm, the average diameter is 274nm, and the length is 1~12cm ( Figure 5 ), the contact between grains is close, and the orientation of adjacent grains is relatively consistent (such as Image 6 shown).

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Abstract

The invention relates to a method for preparing polyvinyl acetate zirconyl precursor sol spinning solution and sub-micron zirconium oxide crystal fibers. The method mainly includes dissolving basic zirconium carbonate, glacial acetic acid, yttrium nitrate hexahydrate and spinning auxiliaries in absolute methanol according to certain proportions to obtain mixed solution and concentrating the mixed solution under reduced pressures at the temperatures of 30-40 DEG C to obtain the colorless, transparent and homogenous polyvinyl acetate zirconyl precursor sol spinning solution; acquiring polyvinyl acetate zirconyl precursor fibers by the aid of electrostatic spinning processes; carrying out pressure resolution on the precursor fibers to remove a ligand which is acetic acid, and then carrying out high-temperature treatment on the precursor fibers in a program-control sintering furnace. The method has the advantages that the diameters of the sub-micron zirconium oxide crystal fibers obtained byte ha id of the method range from 100 nanometers to 2.5 micrometers, and the sub-micron zirconium oxide crystal fibers are excellent in continuity, flexibility and heat-insulation and mechanical properties; the polyvinyl acetate zirconyl precursor sol spinning solution and the sub-micron zirconium oxide crystal fibers can be used at ultrahigh temperatures higher than or equal to 1800 DEG C for a long term.

Description

technical field [0001] The invention relates to a preparation method of poly-zirconyl acetate precursor sol spinning solution and submicron zirconia crystal fiber, and belongs to the field of inorganic non-metallic materials. Background technique [0002] Compared with other oxide fibers that have been widely used, zirconia fibers have a very high melting point (2715°C), the lowest thermal conductivity, high chemical stability, excellent oxidation resistance and extreme acid and alkali corrosion resistance. sex. Zirconia fiber is currently the only crystal fiber material that can meet the ultra-high temperature oxidation atmosphere above 1800 °C. Therefore, the development of zirconia crystal materials for long-term use in ultra-high temperature environments is an urgent need in the fields of aviation, aerospace and ultra-high temperature furnaces. [0003] The applicant started the research on zirconia fiber in 1998, and has obtained a series of patents on zirconia crysta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F9/08D01D5/00
CPCD01D5/0015D01F9/08
Inventor 许东王新强刘雪松朱陆益张光辉
Owner 山东德艾普节能材料有限公司
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