Liquid-state alkane back flow method for preparing nanometer tungsten carbide

A liquid alkane and nanotechnology, applied in the direction of carbides, tungsten/molybdenum carbides, etc., can solve the problems of difficult carbon encapsulation, large shrinkage, high cost, etc., and achieve simple recovery and purification regeneration equipment, simple heat treatment equipment, and easy industrialization The effect of homework

Inactive Publication Date: 2012-08-29
SICHUAN UNIV
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Problems solved by technology

However, these two methods still have defects in varying degrees: the sol-gel method, the raw material is easily hydrolyzed, the shrinkage is large during drying, the cost is high, the yield is low, and the process is cumbersome; the gaseous alkane cracking carbon encapsulation method requires high equipment requirements and consumes The energy is large, it is difficult to achieve carbon encapsulation in a monodisperse state, the prepared WC grains are too large, and the product purity is low, which also limits the application of these two methods to a certain extent.

Method used

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  • Liquid-state alkane back flow method for preparing nanometer tungsten carbide

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example 1

[0031] (1) raw materials: liquid alkane mixture (C 11 -C 16 )5000ml, absolute ethanol 5000ml, hydrated WO 3 About 50g.

[0032] (2) Reflux: 50g hydrated WO 3 Reflux with 500ml of absolute ethanol at 70°C for one hour, then filter; mix the obtained precipitate with fresh 500ml of absolute ethanol, and reflux at 70°C for one hour again, repeat the above reflux process 5 times; then filter the obtained The precipitate and 500ml liquid alkane mixture (C 11 -C 16 ) first reflux at 120°C for 48 hours, then filter the powder, repeatedly extract the ethanol in the alkane filtrate with distilled water, and then add an appropriate amount of anhydrous CaCl to the filtrate 2 Remove the remaining water to obtain a reusable alkane mixture, mix the regenerated liquid alkane mixture with the filtered powder and reflux at 150°C for 48 hours, use the same method as above to obtain a recycled alkane mixture, and then Reflux at 180°C and 210°C for 48 hours respectively, and finally filter o...

example 2

[0038] (1) raw materials: liquid alkane mixture (C 11 -C 16 )5000ml, absolute ethanol 5000ml, hydrated WO 3 About 80g.

[0039] (2) Reflux: 80g hydrated WO 3 Reflux with 500ml of absolute ethanol at 85°C for one hour, and then filter; the obtained precipitate is mixed with fresh 500ml of absolute ethanol, and reflux at 85°C for one hour again, and the above reflux process is repeated 5 times; then filter the obtained The precipitate and 500ml liquid alkane mixture (C 11 -C 16 ) first reflux at 120°C for 24 hours, then filter the powder, repeatedly extract the ethanol in the alkane filtrate with distilled water, and then add an appropriate amount of anhydrous CaCl to the filtrate 2 Remove the remaining water to obtain a reusable alkane mixture, mix the regenerated liquid alkane mixture with the filtered powder and reflux at 150°C for 48 hours, use the same method as above to obtain a recycled alkane mixture, and then Reflux at 180° C. and 210° C. for 48 hours respectively...

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Abstract

The invention relates to a method for preparing nanometer tungsten carbide powder from liquid-state alkane through back flow carbon covering. Sodium tungstate is used as a tungsten source, and a liquid-state alkane mixture (C11 to C16) is used as a carbon source. The invention has the sequential process steps of material preparation, back flow, drying, material charging, high-temperature heat treatment and sampling. The back flow time and the back flow temperature of raw materials are controlled, precursor powder with different carbon contents can be prepared, and high-purity nanometer tungsten carbide powder can be prepared through the heat treatment process. The tungsten carbide powder prepared by the method has the average granularity between 30 and 60 nm and the average grain finenessnumber between 20 and 30 nm. The method of the invention has simple process and lower cost. Compared with an ordinary heat reducing method, the invention saves energy sources, and can easily realize the scale preparation.

Description

technical field [0001] The invention belongs to the field of hard alloy and catalyst material preparation, and in particular relates to a preparation method for preparing tungsten carbide nano powder with a novel organic-inorganic composite precursor. Background technique [0002] In recent years, transition group metal carbides have aroused great interest of researchers due to their important scientific value and potential huge application prospects, and people are competing to use different ideas to synthesize such carbides. [0003] WC is one of the most important materials in transition metal carbides. It has excellent properties such as high melting point, hardness, thermal stability and mechanical stability. It is widely used in the production of cemented carbide materials, in cermets, machining, metallurgy There are important applications in mining, aerospace and other fields. In addition, since the surface electronic structure of WC is similar to that of Pt, it has ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/34C01B32/949
Inventor 姚亚东尹光福李永弟刘飞张皓廖晓明黄忠兵康云清
Owner SICHUAN UNIV
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