WO2012139409A1 - 一种防止合金烧制后粘连和氧化的钒氮合金制备方法 - Google Patents

一种防止合金烧制后粘连和氧化的钒氮合金制备方法 Download PDF

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WO2012139409A1
WO2012139409A1 PCT/CN2012/000148 CN2012000148W WO2012139409A1 WO 2012139409 A1 WO2012139409 A1 WO 2012139409A1 CN 2012000148 W CN2012000148 W CN 2012000148W WO 2012139409 A1 WO2012139409 A1 WO 2012139409A1
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vanadium
reducing agent
alloy
carbon reducing
oxidation
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PCT/CN2012/000148
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English (en)
French (fr)
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郑建伟
应忠芳
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Zheng Jianwei
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Priority to EP12771388.1A priority Critical patent/EP2698344B1/en
Priority to CA2833058A priority patent/CA2833058C/en
Priority to AU2012243313A priority patent/AU2012243313C1/en
Priority to JP2014504144A priority patent/JP5905569B2/ja
Publication of WO2012139409A1 publication Critical patent/WO2012139409A1/zh
Priority to US14/049,242 priority patent/US9227847B2/en

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • C01B21/0615—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium
    • C01B21/0617—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium with vanadium, niobium or tantalum
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/10—Alloys containing non-metals
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/16—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on nitrides
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C5/00—Alloys based on noble metals
    • C22C5/02—Alloys based on gold
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C5/00—Alloys based on noble metals
    • C22C5/04—Alloys based on a platinum group metal
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C5/00—Alloys based on noble metals
    • C22C5/06—Alloys based on silver
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/25—Process efficiency

Definitions

  • the invention relates to the technical field of steel metallurgy, and relates to a preparation method of a vanadium nitrogen alloy for preventing adhesion and oxidation of an alloy after firing.
  • Vanadium-nitrogen alloy is a new type of alloy additive that can replace ferrovanadium for the production of microalloyed steel.
  • the addition of vanadium nitride to steel improves the comprehensive mechanical properties of steel such as strength, toughness, ductility and thermal fatigue resistance, and provides good ductility for steel.
  • the addition of vanadium nitride saves 30-40% of the vanadium addition, which in turn reduces the cost.
  • Another method is a vertical kiln for medium frequency induction heating, such as a method and a device for preparing a vanadium-nitrogen alloy disclosed in the Chinese invention patent application (Application No.: 200710071142.7, application date: 2007-09-20), which is pentoxide Vanadium or vanadium pentoxide and carbonaceous catalyst or graphite as raw materials, made into spherical material, added to medium frequency induction furnace, in nitrogen atmosphere 10M 3 /1H, temperature rise 1350 ° C ⁇ 100 ° C, reduction 2.5-3.5H,
  • the vanadium-nitrogen alloy produced in fact, this method has not been able to achieve continuous production, because all the materials of the vanadium-nitrogen alloy product are stuck together after sintering, so that the material can not automatically go down to the storage chamber, which leads to production.
  • the process can not be continuous, and only one furnace can be produced intermittently. When feeding once, the process of heating and cooling is repeated, the production cost is high, the energy consumption is high
  • an object of the present invention is to provide a method for preparing a vanadium-nitrogen alloy which prevents adhesion and oxidation of an alloy after firing, which can continuously feed and discharge, greatly reducing production cost and improving production. effectiveness.
  • a method for preparing a vanadium-nitrogen alloy for preventing adhesion and oxidation of an alloy after firing comprising the steps of:
  • the vanadium compound, the binder and the premixed carbon reducing agent are mixed and pressed into a raw material ball having a diameter of 30 to 60 mm, and the vanadium compound, the binder and the premixed carbon reducing agent are expressed as the weight of the vanadium compound as follows: 100 parts of vanadium compound, 15 ⁇ 30 parts of premixed carbon reducing agent, 3 ⁇ 12 parts of binder, natural ball is naturally dried; the vanadium compound is vanadium pentoxide or vanadium pentoxide;
  • the raw ball and the granular carbon reducing agent are mixed and continuously put into the vertical kiln of the medium frequency induction furnace.
  • the granular carbon reducing agent is 30 ⁇ 100 parts, and the high purity nitrogen gas is introduced, and the furnace maintains a micro positive pressure of 0.01 ⁇ 0.03MPa, once every 6 ⁇ 8 hours, once, three stages, dry, carbonitrile, cooling, drying section temperature is 100 ⁇ 600°C, and carbonitrile stage temperature is 900 ⁇ 1350 ° C, the cooling section is cooled to below 100 ° C to discharge.
  • the premixed carbon reducing agent is one or more selected from the group consisting of graphite powder and carbon powder.
  • the above particulate carbon reducing agent is one or more selected from the group consisting of granular activated carbon, waste carbon rod, and high quality graphite recarburizing agent.
  • the particle diameter of the above granular activated carbon is 2 ⁇
  • the invention adopts the above technical scheme, and adopts adding a granular carbon reducing agent at the time of feeding, so that one raw ball is separated by a granular carbon reducing agent, on the one hand, the heat transfer property is increased, The temperature is increased faster, and the electricity cost is saved. Since the balls are separated one by one, the continuous feeding and discharging can be achieved, the production cost is greatly reduced, and the production efficiency is improved.
  • a coarse block having a diameter of 50 mm ⁇ 0.5 mm was prepared by a high-pressure ball press, and naturally dried for 3-5 days.
  • the dried raw ball is mixed with 80kg of granular activated carbon with a particle size of 2 ⁇ 4mm, and then added to the medium frequency induction furnace through the automatic feeding system, and then heated into the middle end medium induction furnace through the upper end furnace body, and simultaneously The cooling end is fed with 99.999% nitrogen at 14M 3 /h.
  • the temperature of the middle end furnace material is displayed at 1200 °C ⁇ 100 °C by infrared thermometer.
  • a coarse block having a diameter of 50 mm ⁇ 0.5 mm was prepared by a high-pressure ball press, and naturally dried for 3-5 days. Firstly, the dried raw pellets are mixed with 50kg of granular activated carbon with a particle size of 4 ⁇ 8 mm, and then added to the intermediate frequency induction furnace through the automatic feeding system, and then heated into the middle-end medium frequency induction furnace through the upper end furnace body, and simultaneously 99.999% nitrogen gas is introduced into the cooling end at 8M 3 /h.
  • the temperature of the middle end furnace material is displayed at 1200 °C ⁇ 100 °C by infrared thermometer, and the reaction is carried out for 3.5 hours, so that the material is automatically discharged to the storage cooling chamber.
  • the cooling chamber is jacketed with water and cooled. Finally, the material is discharged through the automatic discharge system.
  • the raw balls and granular activated carbon were added from the automatic feed system at intervals of 3.5 hours.
  • the temperature of the upper end of the second feed is 600 ⁇ 750 ° C. Continuous production, product V: 78.8%, N: 16.5%, C: 1.4%.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Description

一种防止合金烧制后粘连和氧化的钒氮合金制备方法 技术领域
本发明涉及钢铁冶金技术领域， 涉及一种防止合金烧制后粘连和氧化 的钒氮合金制备方法。
背景技术
钒氮合金是一种新型合金添加剂， 可以替代钒铁用于微合金化钢的生 产。 氮化钒添加于钢中能提高钢的强度、 韧性、 延展性及抗热疲劳性等综 合机械性能， 并使钢具有良好的可悍性。 在达到相同强度下， 添加氮化钒 节约钒加入量 30-40%, 进而降低了成本。
现在市场上的钒氮合金生产方法和设备主要有两种， 一种是采用推板 窑连续生产钒氮合金的方法， 此种方法设备投资大， 电能损耗大， 不能即 停即开， 一停下来降温一个月， 维修要一个多月时间， 一开始生产升温也 要一个月时间 ， 差不多一年只能开 8个月时间， 效率低下。 另一种采用的 是中频感应加热的立窑， 如中国发明专利申请（申请号： 200710071142.7 ， 申请日： 2007-09-20)公开的一种钒氮合金制备方法及设备， 该方法以五氧 化二钒或三氧化二钒与碳质催化剂或石墨为原料， 制成球状物料， 加入中 频感应炉中， 在氮气氛 10M3/1H， 升温 1350°C±100°C， 还原 2.5-3.5H, 制 取的钒氮合金， 而事实上这种方法一直不能做到连续生产， 由于在烧结后 钒氮合金产品所有的料全部粘连在一起， 使得料没办法自动下到储料室， 这样导致生产过程不能连续化， 只能一炉出一炉间歇式生产， 投料一次就 要重复升温降温的过程， 生产成本高， 能耗高， 效率低下。 发明内容
为了解决上述的技术问题， 本发明的目的是提供一种防止合金烧制后 粘连和氧化的钒氮合金制备方法， 该方法能够做到连续进料出料， 大大降 低了生产成本， 提高了生产效率。
为了实现上述的目的， 本发明采用了以下的技术方案：
一种防止合金烧制后粘连和氧化的钒氮合金制备方法， 该方法包括以 下的步骤：
( 1 ) 将钒化合物、 粘接剂及预混碳还原剂混合后压制成直径为 30〜 60mm生料球，钒化合物、粘接剂和预混碳还原剂按钒化合物重量份数计如 下： 钒化合物 100份， 预混碳还原剂 15〜30份， 粘接剂 3〜 1 2份， 生料 球自然凉干； 上述的钒化合物选用五氧化二钒或三氧化二钒；
(2) 生料球和颗粒状碳还原剂混合后连续投入到中频感应炉的立窑 中，颗粒状碳还原剂为 30〜100份，通入高纯氮气，炉内保持微正压 0.01〜 0.03MPa, 过 6~8小时投料一次， 出料一次， 分三个阶段， 分别为干燥、 碳 化氮化、 冷却， 干燥段温度为 100~600°C， 碳化氮化阶段温度为 900〜 1350 °C， 冷却段冷却至 100°C以下出料。
作为优选， 上述的预混碳还原剂选用石墨粉、 碳粉中的一种或多种。 作为优选， 上述的颗粒状碳还原剂选用颗粒活性碳、 废炭棒， 优质石 墨增碳剂中的一种或多种。 作为再优选， 上述的颗粒活性碳的粒径为 2〜
10mm。
本发明由于采用了上述的技术方案， 采用在投料时添加颗粒状碳还原 剂， 使一个一个的生料球用颗粒状碳还原剂隔开， 一方面增加了传热性， 使升温更快， 节省电费， 由于烧好的球一个个分开， 能够做到连续进料出 料， 大大降低了生产成本， 提高了生产效率。
具体实施方式
下面对本发明的具体实施方式做进一步说明。
实施例 1
将 100kg98%粉状五氧化二钒与 100目的石墨粉 22kg再加 6kg粘接料 混合均匀后，用高压压球机制成直径 50mm± 0.5mm左右的粗块， 自然干燥 3-5天后投料。首先将凉干后的生料球与 80kg粒径为 2〜4mm颗粒活性碳 混合后通过自动进系统加到中频感应炉中， 经上端炉体预热后进入中端中 频感应炉加热， 同时从冷却端以 14M3/h通入 99.999%的氮气， 中端炉体物 料温度通过红外测温仪显示在 1200°C ± 100°C， 反应 4小时， 使物料自动下 到贮料冷却室， 冷却室带夹套用水冷却。 最后通过自动出料系统出料。 相 隔 4小时， 从自动进料系统加进生料球和颗粒活性碳。 第二次进料上端炉 体温度在 400〜650°C.连续生产，可以得到产品 V:77.8%， N:14.5%, C:2.4%。 实施例 2
将 100kg98%粉状三氧化二钒与 100目的石墨粉 20kg再加 4kg粘接料 混合均匀后，用高压压球机制成直径 50mm±0.5mm左右的粗块， 自然干燥 3-5天后投料。首先将凉干后的生料球与 50kg粒径为 4〜 8 mm颗粒活性 碳混合后通过自动进系统加到中频感应炉中， 经上端炉体预热后进入中端 中频感应炉加热， 同时从冷却端以 8M3/h通入 99.999%的氮气， 中端炉体物 料温度通过红外测温仪显示在 1200 °C ± 100 °C， 反应 3.5小时， 使物料自动 下到贮料冷却室， 冷却室带夹套用水冷却。 最后通过自动出料系统出料。 相隔 3.5小时， 从自动进料系统加进生料球和颗粒活性碳。第二次进料上端 炉体温度在 600〜750°C .连续生产， 可以得到产品 V:78.8%， N:16.5%, C: 1.4%。

Claims

权利要求书
1. 一种防止合金烧制后粘连和氧化的钒氮合金制备方法， 其特征在于该方 法包括以下的步骤：
( 1 ) 将钒化合物、 粘接剂及预混碳还原剂混合后压制成直径为 30〜 60mm生料球，钒化合物、粘接剂和预混碳还原剂按钒化合物重量 份数计如下： 钒化合物 100份， 预混碳还原剂 15〜30份， 粘接剂 3〜8份， 生料球自然凉干； 钒化合物选用五氧化二钒或三氧化二 钒；
(2) 生料球和颗粒状碳还原剂混合后连续投入到中频感应炉的立窑 中， 颗粒状碳还原剂为 30〜100份， 通入高纯氮气， 炉内保持微 正压 0.01〜0.03MPa， 过 6~8小时投料一次， 出料一次， 分三个阶 段， 分别为干燥、 碳化氮化、 冷却， 干燥段温度为 100~600°C，碳 化氮化阶段温度为 900〜1350°C， 冷却段冷却至 100°C以下出料。
2. 根据权利要求 1所述的一种防止合金烧制后粘连和氧化的钒氮合金制备 方法， 其特征在于： 预混碳还原剂选用石墨粉、 碳粉中的一种或多种。
3. 根据权利要求 1所述的一种防止合金烧制后粘连和氧化的钒氮合金制备 方法， 其特征在于： 颗粒状碳还原剂选用颗粒活性碳、 废炭棒、 优质石 墨增碳剂的一种或多种。
4. 根据权利要求 1或 3所述的一种防止合金烧制后粘连和氧化的钒氮合金 制备方法， 其特征在于： 颗粒状碳还原剂的粒径为 2〜10mm。
PCT/CN2012/000148 2011-04-12 2012-02-06 一种防止合金烧制后粘连和氧化的钒氮合金制备方法 WO2012139409A1 (zh)

Priority Applications (5)

Application Number Priority Date Filing Date Title
EP12771388.1A EP2698344B1 (en) 2011-04-12 2012-02-06 Post-sinter conglutination and oxidation-preventative vanadium-nitrogen alloy preparation method
CA2833058A CA2833058C (en) 2011-04-12 2012-02-06 Post-sinter conglutination and oxidation-preventative vanadium-nitrogen alloy preparation method
AU2012243313A AU2012243313C1 (en) 2011-04-12 2012-02-06 Post-sinter conglutination and oxidation-preventative vanadium-nitrogen alloy preparation method
JP2014504144A JP5905569B2 (ja) 2011-04-12 2012-02-06 バナジウム窒素合金の調製方法
US14/049,242 US9227847B2 (en) 2011-04-12 2013-10-09 Method for preparing vanadium-nitrogen alloy

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CN2011100902416A CN102168191B (zh) 2011-04-12 2011-04-12 一种防止合金烧制后粘连和氧化的钒氮合金制备方法

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CN103388096A (zh) * 2012-05-07 2013-11-13 简刚 钒氮合金的生产方法
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