CN104862518A - Method for preparing nitrided ferrovanadium by using vacuum furnace - Google Patents

Method for preparing nitrided ferrovanadium by using vacuum furnace Download PDF

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Publication number
CN104862518A
CN104862518A CN201510187773.XA CN201510187773A CN104862518A CN 104862518 A CN104862518 A CN 104862518A CN 201510187773 A CN201510187773 A CN 201510187773A CN 104862518 A CN104862518 A CN 104862518A
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vacuum oven
vacuum
nitrogen
vacuum furnace
parts
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CN201510187773.XA
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张平俊
张元春
殷永祥
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Sichuan Zhanxiang Special Alloy Technical Ltd Co
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Sichuan Zhanxiang Special Alloy Technical Ltd Co
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Abstract

The invention discloses a method for preparing nitrided ferrovanadium by using a vacuum furnace. A material is pretreated to realize quick heating in the vacuum furnace and to finish the drying, the carbonization and the nitriding within 7-8 hours, so that the time is effectively saved, and the production cost is largely reduced while the production efficiency of the vacuum furnace is improved. The method is used for preparing a nitrided ferrovanadium alloy to achieve the advantages of simple operation, low cost, accurate process control, stable product production and no environmental pollution. The vanadium content of the prepared nitrided ferrovanadium alloy is more than 45%, the nitrogen content can be more than 9%, and the impurity content is low.

Description

A kind of method utilizing vacuum oven to prepare ferrovanadium nitride
Technical field
The present invention relates to field of chemical metallurgical technology, particularly relate to a kind of method utilizing vacuum oven to prepare ferrovanadium nitride.
Background technology
Ferrovanadium nitride is a kind of novel VN alloy additive, performance is better than vanadium iron and vanadium nitride, can be widely used in the product such as high strength spiral shell mosquito reinforcing bar, high-strength line-pipe steel, high strength shaped steel (H profile steel, joist steel, channel-section steel, angle steel), CSP high-strength steel strip, non-hardened and tempered steel, rapid tool steel.Ferrovanadium nitride can reach more than 5.0g/cm3 because of its proportion, than adding vanadium nitride (proportion about 3.5), there is higher specific absorption, the rate of recovery of ferrovanadium nitride can reach more than 95%, average specific VN alloy specific absorption is high by 3% ~ 5%, performance is more stable, has higher crystal grain thinning and promotes the functions such as intensity, toughness, ductility.
Ferrovanadium nitride V/N is about 4.0, is more satisfactory VN alloy additive.A large amount of real application data shows, reaching under the comprehensive mechanical performances such as same intensity, toughness, ductility and thermal fatigue resistance, the Mechanical Fluctuation value of other vanadium alloy steel of ratio interpolation is little, mechanical property minimum value is high, add ferrovanadium nitride ratio and add other vanadium iron saving vanadium 30 ~ 40%, vanadium more than 10% is saved than adding VN alloy, thus reduce steel product cost, be therefore subject to user and extensively welcome.Add ferrovanadium nitride substantially identical with straight carbon steel, simple to operate on smelting, continuous casting, rolling technology, be easy to control, and the strain aging phenomenon of steel can be eliminated.
At present, the production method of ferrovanadium nitride alloy is mainly by after vanadium iron pulverizing, high pressure nitrogen is passed in autoclave, ferrovanadium nitride is prepared through between self-propagating combustion reaction reduction post-heating to 1400 DEG C ~ 1600 DEG C, preparation process requires harsher to apparatus structure, and under high temperature, high pressure, reaction safety is poor.In addition, domestic also have some to utilize barium oxide to carry out the research of the preparation of VN alloy, but these methods to be difficult to realize the preparation of industrialization time longer, generally more than 20 hours, just can complete the flow processs such as intensification, drying, carbonization, nitrogenize.
Summary of the invention
The object of the invention is to the defect overcoming cured fish technology, thering is provided a kind of is raw material with Vanadium Pentoxide in FLAKES, nitridation sintered method is adopted to produce the method for ferrovanadium nitride alloy in a vacuum furnace, produce ferrovanadium nitride alloy by method of the present invention, simple to operate, cost is low, technology controlling and process is accurate, products production is stablized, and environmentally safe, obtained ferrovanadium nitride alloy content of vanadium more than 45%, nitrogen content can reach more than 9%, and foreign matter content is low.
The technical solution used in the present invention is:
Utilize vacuum oven to prepare a method for ferrovanadium nitride, comprise following steps:
A vanadium pentoxide powder is added graphite reduction agent, polyvinyl alcohol adhesive, iron powder by () in proportion, wherein weight ratio is: Vanadium Pentoxide in FLAKES 100 parts, graphite reduction agent 20 parts, polyvinyl alcohol adhesive 10 parts, iron powder 46 parts;
B the material prepared is put into whipping device and is mixed by (), put into pair roller type pressure ball equipment afterwards, material is pressed into oblate spheroid shape, and carries out dry pre-treatment to oblate spheroid shape material;
C pretreated oblate spheroid shape material is positioned in graphite material frame by (), be pushed in vacuum oven by graphite material frame with special-purpose loading device, and airtight vacuum stove;
D () starts vacuum pump, vacuum tightness in vacuum oven is evacuated to below 100Pa;
E () is rapidly heated, make the temp. in vacuum furnace reach 1350 DEG C in 5 hours, then stops vacuumizing;
F () passes into high pure nitrogen (purity >=99.99%) in vacuum oven, take into account by-pass valve control regulate fill rate at 15 ~ 20m3/min by flow, and in final control vacuum oven, atmosphere pressures is 0.05Mpa; Continue while inflated with nitrogen slowly to heat up, time in 1h, the temp. in vacuum furnace rises to 1400 DEG C;
G (), under aforementioned temperature and pressure condition, carries out degree of depth carburizing reagent and nitrogenizing reaction, reaction times 2h;
H () stops heating, continue to fill nitrogen in vacuum oven, when temperature reaches 200 DEG C, stops, for nitrogen, opening vacuum oven, takes out graphite material frame, be cooled to room temperature and obtain ferrovanadium nitride alloy.
Further, content >=97.5% of Vanadium Pentoxide in FLAKES in described step (a), fineness≤80 order, Shi Mo grain degree≤60 order.
The invention has the beneficial effects as follows:
The present invention, by carrying out pre-treatment to material, makes it achieve in a vacuum furnace and is rapidly heated, and drying, carbonization, nitrogenize was accomplished in 7 ~ 8 hours, has effectively saved the time, while raising vacuum oven production efficiency, significantly reduces production cost.Produce ferrovanadium nitride alloy by method of the present invention, simple to operate, cost is low, technology controlling and process is accurate, and products production is stablized, and environmentally safe.Obtained ferrovanadium nitride alloy content of vanadium more than 45%, nitrogen content can reach more than 9%, and foreign matter content is low.
Embodiment
In order to make the advantage of object of the present invention and technical scheme clearly understand, below in conjunction with example, the present invention is further elaborated.
Utilize vacuum oven to prepare a method for ferrovanadium nitride, comprise following steps:
A () is by vanadium pentoxide powder (content >=97.5%, fineness≤80 order) add graphite reduction agent (Li Du≤60 order in proportion), polyvinyl alcohol adhesive, iron powder, wherein weight ratio is: Vanadium Pentoxide in FLAKES 100 parts, graphite reduction agent 20 parts, polyvinyl alcohol adhesive accounts for 10 parts, iron powder 46 parts;
B the material prepared is put into whipping device and is mixed by (), put into pair roller type pressure ball equipment afterwards, material is pressed into oblate spheroid shape, and carries out dry pre-treatment to oblate spheroid shape material;
C pretreated oblate spheroid shape material is positioned in graphite material frame by (), be pushed in vacuum oven by graphite material frame with special-purpose loading device, and airtight vacuum stove;
D () starts vacuum pump, vacuum tightness in vacuum oven is evacuated to below 100Pa;
E () is rapidly heated, make the temp. in vacuum furnace reach 1350 DEG C in 5 hours, then stops vacuumizing;
F () passes into high pure nitrogen (purity >=99.99%) in vacuum oven, take into account by-pass valve control regulate fill rate at 15 ~ 20m3/min by flow, and in final control vacuum oven, atmosphere pressures is 0.05Mpa; Continue while inflated with nitrogen slowly to heat up, time in 1h, the temp. in vacuum furnace rises to 1400 DEG C;
G (), under aforementioned temperature and pressure condition, carries out degree of depth carburizing reagent and nitrogenizing reaction, reaction times 2h;
H () stops heating, continue to fill nitrogen in vacuum oven, when temperature reaches 200 DEG C, stops, for nitrogen, opening vacuum oven, takes out graphite material frame, be cooled to room temperature and obtain ferrovanadium nitride alloy.
The present invention, by carrying out pre-treatment to material, makes it achieve in a vacuum furnace and is rapidly heated, and drying, carbonization, nitrogenize was accomplished in 7 ~ 8 hours, has effectively saved the time, while raising vacuum oven production efficiency, significantly reduces production cost.Produce ferrovanadium nitride alloy by method of the present invention, simple to operate, cost is low, technology controlling and process is accurate, and products production is stablized, and environmentally safe.Obtained ferrovanadium nitride alloy content of vanadium more than 45%, nitrogen content can reach more than 9%, and foreign matter content is low.

Claims (2)

1. utilize vacuum oven to prepare a method for ferrovanadium nitride, it is characterized in that comprising following steps:
A vanadium pentoxide powder is added graphite reduction agent, polyvinyl alcohol adhesive, iron powder by () in proportion, wherein weight ratio is: Vanadium Pentoxide in FLAKES 100 parts, graphite reduction agent 20 parts, polyvinyl alcohol adhesive 10 parts, iron powder 46 parts;
B the material prepared is put into whipping device and is mixed by (), put into pair roller type pressure ball equipment afterwards, material is pressed into oblate spheroid shape, and carries out dry pre-treatment to oblate spheroid shape material;
C pretreated oblate spheroid shape material is positioned in graphite material frame by (), be pushed in vacuum oven by graphite material frame with special-purpose loading device, and airtight vacuum stove;
D () starts vacuum pump, vacuum tightness in vacuum oven is evacuated to below 100Pa;
E () is rapidly heated, make the temp. in vacuum furnace reach 1350 DEG C in 5 hours, then stops vacuumizing; F () passes into high pure nitrogen (purity >=99.99%) in vacuum oven, take into account by-pass valve control regulate fill rate at 15 ~ 20m3/min by flow, and in final control vacuum oven, atmosphere pressures is 0.05Mpa; Continue while inflated with nitrogen slowly to heat up, time in 1h, the temp. in vacuum furnace rises to 1400 DEG C;
G (), under aforementioned temperature and pressure condition, carries out degree of depth carburizing reagent and nitrogenizing reaction, reaction times 2h;
H () stops heating, continue to fill nitrogen in vacuum oven, when temperature reaches 200 DEG C, stops, for nitrogen, opening vacuum oven, takes out graphite material frame, be cooled to room temperature and obtain ferrovanadium nitride alloy.
2. a kind of method utilizing vacuum oven to prepare ferrovanadium nitride according to claim 1, is characterized in that: content >=97.5% of Vanadium Pentoxide in FLAKES in described step (a), fineness≤80 order, Shi Mo grain degree≤60 order.
CN201510187773.XA 2015-04-21 2015-04-21 Method for preparing nitrided ferrovanadium by using vacuum furnace Pending CN104862518A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108048686A (en) * 2017-12-28 2018-05-18 中色(宁夏)东方集团有限公司 A kind of vacuum drying oven prepares ferrovanadium nitride method
CN110938751A (en) * 2019-12-11 2020-03-31 湖南众鑫新材料科技股份有限公司 Method for improving recovery rate of nitrided ferrovanadium

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101289713A (en) * 2007-04-20 2008-10-22 郸城财鑫特种金属有限责任公司 Production process of vanadium-nitrogen alloy
CN102477510A (en) * 2010-11-30 2012-05-30 攀钢集团钢铁钒钛股份有限公司 Method for preparing nitrided ferrovanadium
CN104004934A (en) * 2014-04-30 2014-08-27 四川展祥特种合金科技有限公司 Method for rapid preparation of vanadium-nitrogen alloy

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101289713A (en) * 2007-04-20 2008-10-22 郸城财鑫特种金属有限责任公司 Production process of vanadium-nitrogen alloy
CN102477510A (en) * 2010-11-30 2012-05-30 攀钢集团钢铁钒钛股份有限公司 Method for preparing nitrided ferrovanadium
CN104004934A (en) * 2014-04-30 2014-08-27 四川展祥特种合金科技有限公司 Method for rapid preparation of vanadium-nitrogen alloy

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108048686A (en) * 2017-12-28 2018-05-18 中色(宁夏)东方集团有限公司 A kind of vacuum drying oven prepares ferrovanadium nitride method
CN110938751A (en) * 2019-12-11 2020-03-31 湖南众鑫新材料科技股份有限公司 Method for improving recovery rate of nitrided ferrovanadium

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Application publication date: 20150826