CN100451145C - Vacuum high temperature treatment method for reducing oxygen content of electric dissolving regeneration WC - Google Patents
Vacuum high temperature treatment method for reducing oxygen content of electric dissolving regeneration WC Download PDFInfo
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- CN100451145C CN100451145C CNB2007100349756A CN200710034975A CN100451145C CN 100451145 C CN100451145 C CN 100451145C CN B2007100349756 A CNB2007100349756 A CN B2007100349756A CN 200710034975 A CN200710034975 A CN 200710034975A CN 100451145 C CN100451145 C CN 100451145C
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Abstract
A vacuum and high temperature method for reducing electro regenerated WC oxygen content includes the steps of: putting the electro WC materials in a graphite boat with exhaust holes and a cover while the graphite boat is put in the vacuum heating furnace. When the initial vacuum degree in the furnace reaches 1-10Pa, the temperature in the heating furnace is increased to 1600-2000 degree, which is maintained for 30-120min before the furnace and the materials are cooled to 60 degree and the materials are taken out of the furnace. The vacuum high temperature method in the invention can make the electro regenerated WC oxygen content reach the technical standard of the originally generated WC oxygen content.
Description
Technical field
The present invention relates to the treatment process of the main raw material WC of CEMENTED CARBIDE PRODUCTION, further be meant the vacuum high-temperature treatment process that reduces electric dissolving regeneration WC oxygen level.
Background technology
The main raw material of CEMENTED CARBIDE PRODUCTION is wolfram varbide (WC), and WC forms through wet method and pyrometallurgical processes refinement from tungsten concentrate, is called primary WC.In addition, industrial used hard alloy scraps adopts the molten method of electricity, also can reclaim WC from waste alloy, is called electric dissolving regeneration WC or is called for short electric molten WC.The technical indicator of electric dissolving regeneration WC does not reach the standard of primary WC, mainly be that oxygen level is higher, usually fluctuation is between 0.20-0.40%, for the 5-10 of primary WC (Fei Shi mean particle size range＞14-26 μ m) oxygen level standard 0.04% doubly, cause adopting the Wimet bending strength of electric dissolving regeneration WC production low excessively, in use chipping easily.Therefore, the production of Wimet so far, still with primary WC as main raw material.
Summary of the invention
The technical problem to be solved in the present invention is: higher at the electric dissolving regeneration WC oxygen level that prior art obtains, and do not meet the defective of hard alloy material technical requirements, a kind of vacuum high-temperature treatment process that reduces electric dissolving regeneration WC oxygen level is proposed, it can reduce its oxygen level effectively, makes electric dissolving regeneration WC oxygen level reach the technological standard of primary WC oxygen level.
Technical solution of the present invention is: the molten WC material of electricity is packed into to be provided with venting hole and to add in the graphite boat of top cover, graphite boat is put in the vacuum furnace, when initial depression reaches 1-10Pa in the stove, process furnace just is warming up to 1600 °-2000 ℃, insulation 30-120 branch, material promptly cools to 60 ℃ with the furnace and comes out of the stove.
Below the present invention made further specify.
Vacuum furnace of the present invention can adopt two kinds of equipment: vacuum intermediate frequency furnace and vacuum sintering furnace, two kinds of equipment all can reach described treatment process requirement.Treating processes is: with material (electric molten WC), be loaded on the graphite boat of adding a cover and place in the stove, graphite boat is processed by high-quality graphite blank, and graphite boat is provided with exhaust hole, and new graphite boat needs through the vacuum high-temperature calcination, to remove moisture content and impurity.Initial depression 1-10Pa in the stove adopts 4-7Pa usually, and in high temperature, along with deoxidation Gas body is overflowed and the impurity volatilization, vacuum tightness can descend.Heating temperature is 1600 °-2000 ℃, adopts 1630 °-1850 ℃ usually, low excessively Heating temperature, and material deoxidation deficiency, too high Heating temperature, material seriously lumps.Soaking time 30-120 branch.Usually adopt the 45-60 branch.Heat-up rate does not influence deoxidation effect, rises to Heating temperature in 2-6 hour according to the charge amount may command, and the material tapping temperature should be lower than 60 ℃.
Table 1 has been listed the present invention and has been handled the result that electric dissolving regeneration WC oxygen level changes.
Table 1
Advantage of the present invention is:
1, owing to the tungsten resource shortage, the tungsten concentrate price rises, and utilizing regeneration WC to make Wimet is a desirable approach.The present invention makes electric dissolving regeneration WC oxygen level reach the technological standard of primary WC oxygen level, chooses raw material for the Wimet production, and an alternative leeway is provided.
2, adopt the Wimet of the electric dissolving regeneration WC manufacturing of the present invention's processing, bending strength reaches the technological standard (seeing Table 2) of existing Wimet, satisfies medium level of Wimet and more economic application demand.
Table 2
3, hard alloy material WC all contains trace impurity.The present invention has the effect that reduces electric dissolving regeneration WC impurity simultaneously, makes its quality obtain further to improve.Table 3 has been listed the vacuum intermediate frequency furnace and has been handled electric dissolving regeneration WC, its trace impurity changing conditions.The treatment process parameter is: initial depression 7Pa, 1800 ℃ of Heating temperatures, soaking time 45 minutes.
Table 3
Embodiment
Embodiment 1: equipment is vacuum sintering furnace, and material (electric molten WC) is 200kg altogether, is loaded on 10 graphite boats respectively, and boat is added a cover, and is provided with exhaust hole, and boat is regularly arranged to be placed in the stove.Start vacuum system, vacuum system is made up of mechanical pump and lobe pump, and vacuum tightness reaches 5Pa (initial depression), heat temperature raising rose to 1630 ℃ in 4 hours, was incubated 50 fens, cut off heating current, furnace cooling, vacuum system keep the mechanical pump running, close lobe pump, furnace temperature goes out boat for 60 ℃, material just can sieve through fragmentation slightly, sampling analysis, and oxygen level reduces to 0.033% from 0.28%.
Embodiment 2: equipment is the vacuum intermediate frequency furnace, and material (electric molten WC) is 100kg altogether, is loaded on 10 graphite boats respectively, and boat is added a cover, and is provided with exhaust hole, and boat places in the crystal vessel of intermediate frequency inductor.Start vacuum system, vacuum system is made up of mechanical pump and lobe pump, and vacuum tightness reaches 7Pa (initial depression), heat temperature raising rose to 1800 ℃ in 2 hours, soaking time 45 minutes, cut off heating current, furnace cooling, vacuum system keep the mechanical pump running, close lobe pump, furnace temperature goes out boat for 60 ℃, material sieves through fragmentation, sampling analysis, and oxygen level reduces to 0.039% from 0.35%.
Claims (2)
1, a kind of vacuum high-temperature treatment process that reduces electric dissolving regeneration WC oxygen level, it is characterized in that, this method is: electric dissolving regeneration WC material is packed into to be provided with venting hole and to add in the graphite boat of top cover, graphite boat is put in the vacuum furnace, when initial depression reaches 1-10Pa in the stove, process furnace just is warming up to 1600-2000 ℃, and soaking time 30-120 branch, material promptly cool to 60 ℃ with the furnace and come out of the stove.
According to the vacuum high-temperature treatment process of right 1 described reduction electric dissolving regeneration WC oxygen level, it is characterized in that 2, described initial depression is 4-7Pa, Heating temperature is 1630-1850 ℃, and soaking time is the 45-60 branch.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100349756A CN100451145C (en) | 2007-05-21 | 2007-05-21 | Vacuum high temperature treatment method for reducing oxygen content of electric dissolving regeneration WC |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2007100349756A CN100451145C (en) | 2007-05-21 | 2007-05-21 | Vacuum high temperature treatment method for reducing oxygen content of electric dissolving regeneration WC |
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| Publication Number | Publication Date |
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| CN101054640A CN101054640A (en) | 2007-10-17 |
| CN100451145C true CN100451145C (en) | 2009-01-14 |
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| CNB2007100349756A Expired - Fee Related CN100451145C (en) | 2007-05-21 | 2007-05-21 | Vacuum high temperature treatment method for reducing oxygen content of electric dissolving regeneration WC |
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| CN111500829B (en) * | 2020-04-27 | 2021-10-29 | 厦门钨业股份有限公司 | A method for quenching and recycling waste cemented carbide |
Citations (7)
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| CN1054270A (en) * | 1991-03-19 | 1991-09-04 | 国营自贡硬质合金厂 | The recovery and treatment method of waste hand alloy material |
| US5603781A (en) * | 1995-04-27 | 1997-02-18 | Korea Institute Of Science And Technology | Method for inhibiting the oxidation of hard metal powder |
| CN1236016A (en) * | 1998-05-19 | 1999-11-24 | 自贡硬质合金厂 | Recovering and regenerating treating process for waste hard alloy |
| US6617271B1 (en) * | 2002-03-19 | 2003-09-09 | Vladimir Yurievich Kodash | Tungsten carbide cutting tool materials |
| WO2005023729A1 (en) * | 2003-09-08 | 2005-03-17 | Kraemer Martin | Tungsten carbide cutting tool material |
| CN1827264A (en) * | 2006-03-24 | 2006-09-06 | 自贡市天恒合金应用技术有限公司 | Method for preparing composite raw powder for the production of ultrafine hard alloy |
| CN1843908A (en) * | 2006-04-30 | 2006-10-11 | 北京科技大学 | A kind of preparation method of nanometer tungsten carbide powder |
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2007
- 2007-05-21 CN CNB2007100349756A patent/CN100451145C/en not_active Expired - Fee Related
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1054270A (en) * | 1991-03-19 | 1991-09-04 | 国营自贡硬质合金厂 | The recovery and treatment method of waste hand alloy material |
| US5603781A (en) * | 1995-04-27 | 1997-02-18 | Korea Institute Of Science And Technology | Method for inhibiting the oxidation of hard metal powder |
| CN1236016A (en) * | 1998-05-19 | 1999-11-24 | 自贡硬质合金厂 | Recovering and regenerating treating process for waste hard alloy |
| US6617271B1 (en) * | 2002-03-19 | 2003-09-09 | Vladimir Yurievich Kodash | Tungsten carbide cutting tool materials |
| WO2005023729A1 (en) * | 2003-09-08 | 2005-03-17 | Kraemer Martin | Tungsten carbide cutting tool material |
| CN1827264A (en) * | 2006-03-24 | 2006-09-06 | 自贡市天恒合金应用技术有限公司 | Method for preparing composite raw powder for the production of ultrafine hard alloy |
| CN1843908A (en) * | 2006-04-30 | 2006-10-11 | 北京科技大学 | A kind of preparation method of nanometer tungsten carbide powder |
Non-Patent Citations (4)
| Title |
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| 电溶法再生WC在凿岩纤片合金生产中的应用. 张平.四川有色金属，第无卷第1期. 2007 |
| 电溶法再生WC在凿岩纤片合金生产中的应用. 张平.四川有色金属，第无卷第1期. 2007 * |
| 硬质合金回收利用工艺现状. 翟昕.有色金属再生与利用，第无卷第1期. 2004 |
| 硬质合金回收利用工艺现状. 翟昕.有色金属再生与利用，第无卷第1期. 2004 * |
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