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Preparation method of ultramicro columnar K2Ti6O13 whiskers

A columnar and ultra-fine technology, applied in the field of inorganic fiber materials, can solve the problems of complex whisker processing, long holding time, environmental impact, etc., and achieve the effects of simple process, simple production equipment and convenient operation.

Inactive Publication Date: 2015-04-08
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The holding time of this method is relatively long, and the follow-up treatment of whiskers is relatively complicated, and the large discharge of lye and acid also has an impact on the environment

Method used

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  • Preparation method of ultramicro columnar K2Ti6O13 whiskers
  • Preparation method of ultramicro columnar K2Ti6O13 whiskers
  • Preparation method of ultramicro columnar K2Ti6O13 whiskers

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Heat and melt 30g of stearic acid at 80°C, after it is completely melted, press Ti(OC 2 h 5 ) 4 The / KOH molar ratio is 3:1.1. Add the initial material, that is, add 11ml of 1mol / L KOH aqueous solution while hot while stirring, and control the dropping rate at 30-45 drops / min. At the same time, add ethyl titanate 10.2 to the above system g, continue to stir for 40min, and obtain KOH-Ti(OC 2 h 5 ) 4 Gel; burn off most of the organic matter in the above gel in an electric furnace at 550°C to obtain K 2 Ti 6 o 13 Precursor. After cooling, ball mill for 30 minutes, then heat up to 900°C for 2 hours at a heating rate of 5°C / min, and then cool down with the furnace to obtain the ultrafine columnar K 2 Ti 6 o 13 whiskers.

[0031] The ultrafine columnar K prepared in this embodiment 2 Ti 6 o 13 Whiskers, the process flow is as follows figure 1 , its XRD spectrum and field emission scanning electron photographs are shown in figure 2 , image 3 . Depend on f...

Embodiment 2

[0033] Heat and melt 35g of stearic acid at 90°C, after it is completely melted, press Ti(OC 2 h 5 ) 4 The / KOH molar ratio is 3:1.1. Add the initial material, that is, add 11ml of 1mol / L KOH aqueous solution while hot while stirring, and control the dropping rate at 30-45 drops / min. At the same time, add ethyl titanate 10.2 to the above system g, continue to stir for 60min, and obtain KOH-Ti(OC 2 h 5 ) 4 Gel; burn most of the organic matter in the above gel in an electric furnace at 600°C to obtain K 2 Ti 6 o 13 Precursor. After cooling, ball mill for 30 minutes, then heat up to 950°C at a heating rate of 7°C / min and calcined for 1.5 hours, and the ultrafine columnar K can be obtained after cooling in the furnace. 2 Ti 6 o 13 whiskers.

Embodiment 3

[0035] Heat and melt 32.5g stearic acid at 80°C, after it is completely melted, press Ti(OC 2 h 5 ) 4 The / KOH molar ratio is 3:1.1. Add the initial material, that is, add 11ml of 1mol / L KOH aqueous solution while hot while stirring, and control the dropping rate at 30-45 drops / min. At the same time, add ethyl titanate 10.2 to the above system g, continue to stir for 45min, and obtain KOH-Ti(OC 2 h 5 ) 4 Gel; burn most of the organic matter in the above gel in an electric furnace at 600°C to obtain K 2 Ti 6 o 13 Precursor. After cooling, ball mill for 30 min, then heat up to 850 °C for 3 hours at a heating rate of 6 °C / min to obtain the ultrafine columnar K 2 Ti 6 o 13 whiskers.

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Abstract

The invention relates to a stearic acid method for preparing ultramicro columnar potassium hexatitanate whiskers which have uniform size and favorable crystallization and shape. The whisker diameters are 0.6-0.9 mu m, and the length-to-diameter ratio exceeds 15. The main raw materials are stearic acid, potassium hydroxide, ethyl titanate. The method comprises the following steps: by using low melting point (80 DEG C) and dispersity of stearic acid which is used as a reaction medium, melting reactants in the stearic acid, combusting to remove most organic substances, and roasting at high temperature, wherein the stearic acid is not only used as a dispersant in the synthesis process to mix the reactant raw materials on the molecular level, but also used as a reactant to generate coordination action with K<+> and Ti<4+> in the reactant raw materials. The invention has the characteristics of simple technical operation, low roasting temperature, short reaction time, high purity, favorable degree of crystallization, less product aggregation and the like, and is suitable industrialized large-scale production.

Description

technical field [0001] The invention belongs to the field of inorganic fiber materials, in particular to an ultrafine columnar K 2 Ti 6 o 13 Preparation method of stearic acid for whiskers. Background technique [0002] Potassium titanate whisker is a new type of inorganic material developed by DuPont Company of the United States in 1958. Its composition is K 2 O nTiO 2 (n=1, 2, 4, 6, 8), where potassium hexatitanate ( K 2 Ti 6 o 13 ) belongs to the monoclinic structure, space group C2 / m, and the structure is based on TiO 6 The octahedron is connected by co-planar and common-edge to form a chained tunnel-like structure, K + Ions occupy the middle of the tunnel. Due to this unique structure, K 2 Ti 6 o 13 Has excellent physical and chemical properties, such as excellent corrosion resistance, heat resistance, wear resistance, lubricity, electrical insulation and high infrared reflection, and its high melting point, low density, high tensile strength, Due to its sm...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B29/32C30B29/62C30B5/00
Inventor 吉晓莉吴事江陈卓翟成成王先海
Owner WUHAN UNIV OF TECH
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