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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 the problems of dangerous hydrogen, lack of spinnability, and lack of spinnability of silica-alumina sol

Inactive Publication Date: 2021-10-08
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

[0036] 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, and the molar ratio of aluminum hydroxide to the formic acid added for the second time is 1:0.5. Afterwards, the mixture solution was concentrated at 100° C., continuously stirred and condensed and refluxed, at a temperature of 40° C., and a vacuum of 0.09 MPa to remove the carboxylic acid, and reacted for 10 hours to prepare a transparent aluminum carboxylate solution; the liquid two Silicon oxide and formic acid were mixed at a molar ratio of 1:1, and the precipitate was filtered after ultrasonic dispersion for 30 minutes; lactic acid, glycerin, polyvinyl butyral, and polyvinyl alcohol were added to the clarified liquid for mixing;

[0037] Depend on figure 1 As can be seen from the NMR spectrum of the aluminum carboxylate solution: the prepared aluminum carboxylate solut...

Embodiment 2

[0040] 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, and the molar ratio of aluminum hydroxide to acetic acid is 1:1. Afterwards, the mixture solution was concentrated at 150° C., continuously stirred and condensed and refluxed, at a temperature of 70° C., and a vacuum of 0.09 MPa to remove carboxylic acid, and reacted for 20 hours to prepare a transparent aluminum carboxylate solution; figure 1 The aluminum carboxylate solution NMR spectra can be seen: the prepared aluminum carboxylate solution exists in the form of multimer Al8-18OX12-27. 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).

[0041]Then mix silica sol and acetic acid at a molar ratio of 1:2, ultrasonically disper...

Embodiment 3

[0043] 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 propionic acid and oxalic acid is 1:3, and the molar ratio of aluminum hydroxide to acetic acid is 1:2. Afterwards, the mixture solution was reacted for 30 hours at 200° C. under continuous stirring and condensing and reflux conditions to prepare a transparent aluminum carboxylate solution; by figure 1 The aluminum carboxylate solution NMR spectra can be seen: the prepared aluminum carboxylate solution exists in the form of multimer Al8-18OX12-27. 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).

[0044] Then liquid silicon dioxide and propionic acid were mixed at a molar ratio of 1:3, and the precipitate was filtered after ultrasonic dispersion for 60 minutes; poly...

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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 concentrating and aging to obtain the mullite fibers. According to the invention, in the production process, harmful gases such as chlorine, nitrogen dioxide, sulfur dioxide and the like are not generated, the raw materials are low in requirement and easy to store, commercially available raw materials can be directly used, the technical problem that the commercially available aluminum hydroxide raw material cannot be used for preparing spinnable mullite fibers is solved, and the preparation process is simple and environmentally 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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