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Preparation method of low-cost mullite fiber

A mullite fiber, low-cost technology, applied in the field of low-cost mullite fiber preparation, can solve problems such as extremely high requirement for raw material activity, low activity, lack of spinnability and the like

Pending Publication Date: 2021-12-31
SHANDONG RES & DESIGN ACADEMY OF IND CERAMICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, although aluminum hydroxide is used as an aluminum source to prepare mullite fibers, the process is cumbersome and complicated, and the requirements for the activity of raw materials are extremely high, and the prepared mullite fibers often do not have spinnability.
In most of the processes for preparing spinnable mullite fibers, aluminum hydroxide and silica sol as the main raw materials must be produced and used now, which increases the process flow and preparation costs, and for the existing aluminum hydroxide and silica sol There are quality requirements, and the commercially available aluminum hydroxide will be placed for a long time from the preparation to the market, resulting in a decrease in activity. The silica-alumina sol prepared by using this aluminum hydroxide is not spinnable, so the same commercially available common Raw materials cannot produce satisfactory spinnable sols
[0004] The inorganic aluminum salt method mainly uses aluminum powder and aluminum salt to reflux at high temperature to produce aluminum sol, and then adds silica sol to produce mullite fiber, but dangerous hydrogen gas will be generated during the reaction process, and some aluminum salts containing Cl and N The by-products precipitated during the reaction will also greatly pollute the environment

Method used

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  • Preparation method of low-cost mullite fiber
  • Preparation method of low-cost mullite fiber
  • Preparation method of low-cost mullite fiber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Add formic acid and acetic acid into distilled water at 50°C, stir and mix well before adding aluminum hydroxide powder. The molar ratio of aluminum hydroxide to formic acid and acetic acid is 1:1. Afterwards, the mixture solution was reacted at 100° C. under continuous stirring and reflux for 10 hours, and then concentrated to remove carboxylic acid at a temperature of 40° C. and a vacuum of 0.09 MPa to prepare a transparent aluminum carboxylate solution. Mix liquid silicon dioxide and formic acid at a molar ratio of 1:1, ultrasonically disperse for 30 minutes, and filter the precipitate; add lactic acid, glycerin, polyvinyl butyral, and polyvinyl alcohol to the clarified liquid for mixing to obtain a silicon additive.

[0039] Depend on figure 1 As can be seen from the NMR spectrum of the aluminum carboxylate solution: the prepared aluminum carboxylate solution is based on the polymer Al 8- 18 OX 12-27 form exists. Depend on image 3 The infrared test pattern o...

Embodiment 2

[0042]Add propionic acid and oxalic acid into distilled water at 65°C, stir and mix well before adding aluminum hydroxide powder. The molar ratio of aluminum hydroxide to propionic acid and oxalic acid is 1:2. Afterwards, the mixture solution was reacted at 150° C. under continuous stirring and reflux for 20 hours, and then concentrated to remove carboxylic acid at a temperature of 70° C. and a vacuum of 0.09 MPa to prepare a transparent aluminum carboxylate solution. Depend on figure 1 As can be seen from the NMR spectrum of the aluminum carboxylate solution: the prepared aluminum carboxylate solution is based on the polymer Al 8-18 OX 12-27 form exists. Depend on image 3 The infrared test pattern of the aluminum carboxylate solution shows that the functional groups of its multimer exist in the form of groups such as (HCOO) (RCOO) (OOC-COOH).

[0043] Then mix the silica sol and acetic acid at a molar ratio of 1:2, ultrasonically disperse for 45 minutes, and filter the...

Embodiment 3

[0045] Add malonic acid and citric acid into distilled water at 80°C, stir and mix well, and then add aluminum hydroxide powder. The molar ratio of aluminum hydroxide to malonic acid and citric acid is 1:3. Afterwards, the mixture solution was reacted at 200° C. under continuous stirring and reflux for 30 hours, and then concentrated to remove carboxylic acid at a temperature of 100° C. and a vacuum of 0.1 MPa to prepare a transparent aluminum carboxylate solution. Depend on figure 1 As can be seen from the NMR spectrum of the aluminum carboxylate solution: the prepared aluminum carboxylate solution is based on the polymer Al 8-18 OX 12-27 form exists. Depend on image 3 The infrared test pattern of the aluminum carboxylate solution shows that the functional groups of its multimer exist in the form of groups such as (HCOO) (RCOO) (OOC-COOH).

[0046] Then liquid silicon dioxide and propionic acid were mixed at a molar ratio of 1:3, and the precipitate was filtered after ...

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Abstract

The invention discloses a preparation method of low-cost mullite fibers. The preparation method comprises the following steps: firstly, preparing an aluminum carboxylate solution; preparing a silicon additive; and mixing the aluminum carboxylate solution with the silicon additive, reacting to obtain precursor sol, and performing concentration aging, spinning, heat treatment and the like to obtain the mullite fiber. Harmful gases such as chlorine, nitrogen dioxide and sulfur dioxide are not generated in the production process; the raw materials are low in requirement and easy to store, commercially available raw materials can be directly used, and the technical problem that the commercially available aluminum hydroxide raw materials cannot be used for preparing spinnable mullite fibers is solved. The preparation process is simple, green and environment-friendly.

Description

technical field [0001] The invention belongs to the field of preparation of inorganic nanometer materials, in particular to a preparation method of low-cost mullite fiber. Background technique [0002] Mullite ceramic fiber is an engineering material with excellent comprehensive performance. It can be used as a reinforcing component of ceramics, metals, plastics and other materials. It has the characteristics of high temperature resistance, corrosion resistance, high strength, good thermal shock resistance, and good thermal insulation performance. , plays an important role in the industrial and aerospace fields. [0003] Most of the existing technologies use the sol-gel method and the inorganic aluminum salt method to prepare mullite fibers, and the preparation of the precursor sol in the sol-gel method is the most critical process. In the prior art, although aluminum hydroxide is used as an aluminum source to prepare mullite fibers, the process is cumbersome and complicate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/185C04B35/622D01F9/08
CPCC04B35/185C04B35/62245D01F9/08
Inventor 张铭霞王重海刘振王雪朋齐学礼程之强吕锋何子扬李茹徐浩南
Owner SHANDONG RES & DESIGN ACADEMY OF IND CERAMICS
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