CN106498266B - A kind of preparation method of VN alloy - Google Patents
A kind of preparation method of VN alloy Download PDFInfo
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- CN106498266B CN106498266B CN201611091160.7A CN201611091160A CN106498266B CN 106498266 B CN106498266 B CN 106498266B CN 201611091160 A CN201611091160 A CN 201611091160A CN 106498266 B CN106498266 B CN 106498266B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C35/00—Master alloys for iron or steel
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- 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
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/02—Alloys based on vanadium, niobium, or tantalum
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Abstract
The present invention relates to a kind of preparation method of VN alloy.Its technical scheme is：It is (0.1 ~ 0.3): 1 dispensing in mass ratio by carbonaceous reducing agent and the vanadic sulfate in terms of anhydride, mixes, obtain mixed material.It is lump material by mixed material machine pressure, the density of the lump material is 1.5 ~ 2.0g/cm3；The lump material is dried into 1 ~ 7h under the conditions of 60 ~ 120 DEG C again.Under conditions of normal pressure and nitrogen flow are 100 ~ 600mL/min, dried lump material is heated to 1000 ~ 1400 DEG C, 1 ~ 5h is incubated, cools to room temperature ~ 100 DEG C with the furnace, come out of the stove, obtain VN alloy.The carbonaceous reducing agent is one or more of carbon black, graphite and activated carbon, and the granularity of the carbonaceous reducing agent is 0.074 ~ 0.250mm；The granularity of the vanadic sulfate is 0.074 ~ 0.250mm.The present invention has the characteristics of technique is simple, the reaction time is short low with reaction temperature.
Description
Technical field
The invention belongs to vanadium alloy technical field.More particularly to a kind of preparation method of VN alloy.
Background technology
VN alloy is a kind of new alloy addition, and making an addition in steel can be carried by precipitation strength and refined crystalline strengthening
The comprehensive mechanical performances such as Gao Gang intensity, toughness, ductility, wearability, corrosion resistance and thermal fatigue resistance, it can be effectively improved
The welding performance of steel.Compared with adding vanadium iron in steel, vanadium amount 20 ~ 40% can be saved under the same intensity, so as to reduce
Steel and alloy chemical conversion this.In V-alloyed steel nitrogen content from 40ppm rise to 160ppm when, yield strength increases 110MPa, because
This, improves the nitrogen content in VN alloy, the effectively save rolled steel dosage of energy, can save raw material and smelting cost, have huge
Resources conservation and environmental protection double benefit.
The preparation method of traditional VN alloy is by vanadic anhydride, vanadium tetraoxide, vanadium trioxide, metavanadic acid
Ammonium, ammonium poly-vanadate etc. are used as raw material, with addition of reducing agent, binding agent, accelerator etc., are generated at high temperature with nitrogen or ammonia reaction
Vanadium-nitrogen alloy product.
" a kind of production method of simple vanadium nitride "（CN102173395A）Patented technology, with V2O5It is raw material with graphite powder,
Binding agent polyvinyl alcohol water solution is added after mixing, pressure ball after wet mixing, dries, in 800 DEG C of prereduction 5h or so, is warming up to 1350
DEG C persistently drastic reduction more than 6h and carbonization, more than 99.99% nitrogen is constantly filled with the process；It is continuously heating to
1600 DEG C, the nitridation sintered of 6 ~ 10h is carried out, this pressure process is 0.02MPa, is completed in 20h or so, reaction total time, cooling
Come out of the stove to 150 DEG C, VN alloy is made.
" a kind of method for preparing VN alloy "（CN103952512A）Patented technology, by ammonium metavanadate or/and more vanadic acid
Ammonium reduces 3 ~ 6h under nitrogen and hydrogen mixture atmosphere in 600 ~ 650 DEG C, obtains barium oxide；By obtained barium oxide and catalyst,
Carbonaceous pulvis, binding agent and water wet method ball, 1 ~ 3h are incubated in 300 ~ 350 DEG C under normal pressure blanket of nitrogen, then heat to 1450 ~
1650 DEG C, charged pressure is positive 0.04 ~ 0.08MPa nitrogen, carries out 6 ~ 9h of nitridation reaction, cooling discharge, obtains VN alloy.
" a kind of vanadium nitrogen alloy preparation method "（CN102936678A）Patented technology, vanadium raw materials powder, iron powder, carbonaceous powders will be contained
Agent and binding agent are stirred rear compound stalk forming, then with rice husk by volume 1: 1 ratio be sent into calcining kiln, done under oxygen free condition
Processing is evaporated, temperature is 600 ~ 650 DEG C, and the time is 6 ~ 7h, is then heated to 1300 ~ 1500 DEG C, while is passed through high pure nitrogen, the time
2 ~ 4h, cooling, which is come out of the stove, obtains vanadium nitride product.
Content of nitrogen in vanadium-nitrogen alloy prepared by aforementioned production method is higher, but has the drawback that：Complex process, production week
Phase is grown and preparation temperature is high.
The content of the invention
It is contemplated that overcome prior art defect, it is therefore an objective to provide that a kind of technique is simple, the reaction time is short and reaction temperature
Spend the preparation method of low VN alloy.
To achieve the above object, the technical solution adopted by the present invention comprises the concrete steps that：
Step 1: being (0.1 ~ 0.3): 1 dispensing in mass ratio by carbonaceous reducing agent and the vanadic sulfate in terms of anhydride, mix
It is even, obtain mixed material.
Step 2: it is lump material by mixed material machine pressure, the density of the lump material is 1.5 ~ 2.0g/cm3；
The lump material is dried into 1 ~ 7h under the conditions of 60 ~ 120 DEG C again.
Step 3: under conditions of normal pressure and nitrogen flow are 100 ~ 600mL/min, dried lump material is heated
To 1000 ~ 1400 DEG C, 1 ~ 5h is incubated, room temperature ~ 100 DEG C is cooled to the furnace, comes out of the stove, obtain VN alloy.
The carbonaceous reducing agent is one or more of carbon black, graphite and activated carbon.
The granularity of the carbonaceous reducing agent is 0.074 ~ 0.250mm.
The granularity of the vanadic sulfate is 0.074 ~ 0.250mm.
Due to using above-mentioned technical proposal, the beneficial effects of the invention are as follows：
(1) present invention uses vanadic sulfate as raw material, because vanadic sulfate contains the crystallization water and absorption water, in agglomeration
It is simple without outer adding additives, technique in journey.
(2) vanadic sulfate that the present invention uses decomposes in heating process so that the specific surface area increase of material, adds
With the contact area of nitrogen, reduction nitridation speed is improved, adds nitrogen content, without added promoter and reduction nitridation time
It is short.
(3) reaction temperature of the present invention is low, is advantageous to save energy consumption.
VN alloy prepared by the present invention is after testing：Content of vanadium is 77.52 ~ 80.43wt%；Nitrogen content be 12.67 ~
16.98wt%；Apparent density is 3.03 ~ 3.54g/cm3。
Therefore, the present invention has the characteristics of technique is simple, the reaction time is short low with reaction temperature.
Embodiment
Technical solution of the present invention is further described in detail with reference to embodiment, does not limit the present invention to institute
In the embodiment stated.
Embodiment 1
A kind of preparation method of VN alloy.The technical scheme that the present embodiment uses comprises the concrete steps that：
Step 1: being (0.1 ~ 0.2): 1 dispensing in mass ratio by carbonaceous reducing agent and the vanadic sulfate in terms of anhydride, mix
It is even, obtain mixed material.
Step 2: it is lump material by mixed material machine pressure, the density of the lump material is 1.5 ~ 1.8g/cm3；
The lump material is dried into 1 ~ 7h under the conditions of 60 ~ 120 DEG C again.
Step 3: under conditions of normal pressure and nitrogen flow are 100 ~ 400mL/min, dried lump material is heated
To 1000 ~ 1200 DEG C, 3 ~ 5h is incubated, room temperature ~ 100 DEG C is cooled to the furnace, comes out of the stove, obtain VN alloy.
The carbonaceous reducing agent is carbon black.
The granularity of the carbonaceous reducing agent is 0.074 ~ 0.125mm.
The granularity of the vanadic sulfate is 0.074 ~ 0.125mm.
VN alloy manufactured in the present embodiment is after measured：Content of vanadium is 78.12 ~ 80.43wt%；Nitrogen content be 12.82 ~
14.87wt%；Apparent density is 3.06 ~ 3.36g/cm3。
Embodiment 2
A kind of preparation method of VN alloy.The present embodiment removes carbonaceous reducing agent, and remaining is the same as embodiment 1.
The carbonaceous reducing agent is the mixture of graphite and activated carbon.
VN alloy manufactured in the present embodiment is after measured：Content of vanadium is 78.56 ~ 79.47wt%；Nitrogen content be 12.67 ~
14.92wt%；Apparent density is 3.12 ~ 3.41g/cm3。
Embodiment 3
A kind of preparation method of VN alloy.The technical scheme that the present embodiment uses comprises the concrete steps that：
Step 1: being (0.2 ~ 0.3): 1 dispensing in mass ratio by carbonaceous reducing agent and the vanadic sulfate in terms of anhydride, mix
It is even, obtain mixed material.
Step 2: it is lump material by mixed material machine pressure, the density of the lump material is 1.6 ~ 1.9g/cm3；
The lump material is dried into 1 ~ 7h under the conditions of 60 ~ 120 DEG C again.
Step 3: under conditions of normal pressure and nitrogen flow are 200 ~ 500mL/min, dried lump material is heated
To 1200 ~ 1300 DEG C, 2 ~ 4h is incubated, room temperature ~ 100 DEG C is cooled to the furnace, comes out of the stove, obtain VN alloy.
The carbonaceous reducing agent is graphite.
The granularity of the carbonaceous reducing agent is 0.125 ~ 0.250mm.
The granularity of the vanadic sulfate is 0.125 ~ 0.250mm.
VN alloy manufactured in the present embodiment is after measured：Content of vanadium is 77.92 ~ 79.73wt%；Nitrogen content be 13.65 ~
16.92wt%；Apparent density is 3.09 ~ 3.45g/cm3。
Embodiment 4
A kind of preparation method of VN alloy.The present embodiment removes carbonaceous reducing agent, and remaining is the same as embodiment 3.
The carbonaceous reducing agent is the mixture in carbon black and activated carbon.
VN alloy manufactured in the present embodiment is after measured：Content of vanadium is 77.89 ~ 79.98wt%；Nitrogen content be 14.51 ~
15.99wt%；Apparent density is 3.06 ~ 3.47g/cm3。
Embodiment 5
A kind of preparation method of VN alloy.The technical scheme that the present embodiment uses comprises the concrete steps that：
Step 1: be (0.15 ~ 0.25): 1 dispensing in mass ratio by carbonaceous reducing agent and the vanadic sulfate in terms of anhydride,
Mix, obtain mixed material.
Step 2: it is lump material by mixed material machine pressure, the density of the lump material is 1.7 ~ 2.0g/cm3；
The lump material is dried into 1 ~ 7h under the conditions of 60 ~ 120 DEG C again.
Step 3: under conditions of normal pressure and nitrogen flow are 300 ~ 600mL/min, dried lump material is heated
To 1300 ~ 1400 DEG C, 1 ~ 3h is incubated, room temperature ~ 100 DEG C is cooled to the furnace, comes out of the stove, obtain VN alloy.
The carbonaceous reducing agent is activated carbon.
The granularity of the carbonaceous reducing agent is 0.100 ~ 0.175mm.
The granularity of the vanadic sulfate is 0.100 ~ 0.175mm.
VN alloy manufactured in the present embodiment is after measured：Content of vanadium is 77.52 ~ 79.86wt%；Nitrogen content be 15.31 ~
16.98wt%；Apparent density is 3.10 ~ 3.46g/cm3。
Embodiment 6
A kind of preparation method of VN alloy.The present embodiment removes carbonaceous reducing agent, and remaining is the same as embodiment 5.
The carbonaceous reducing agent is the mixture of carbon black and graphite.
VN alloy manufactured in the present embodiment is after measured：Content of vanadium is 77.81 ~ 79.62wt%；Nitrogen content be 14.39 ~
16.91wt%；Apparent density is 3.03 ~ 3.54g/cm3。
Embodiment 7
A kind of preparation method of VN alloy.The present embodiment removes carbonaceous reducing agent, and remaining is the same as embodiment 5.
The carbonaceous reducing agent is the mixture in carbon black, graphite and activated carbon.
VN alloy manufactured in the present embodiment is after measured：Content of vanadium is 78.12 ~ 79.89wt%；Nitrogen content be 14.76 ~
16.03wt%；Apparent density is 3.11 ~ 3.48g/cm3。
The beneficial effect of present embodiment is：
(1) present embodiment using vanadic sulfate be used as raw material, due to vanadic sulfate contain the crystallization water and adsorb water,
It is simple without outer adding additives, technique during agglomeration.
(2) vanadic sulfate that present embodiment uses decomposes in heating process so that the specific surface area of material increases
Greatly, the contact area with nitrogen is added, reduction nitridation speed is improved, adds nitrogen content, without added promoter and also
Former nitridation time is short.
(3) present embodiment reaction temperature is low, is advantageous to save energy consumption.
VN alloy prepared by present embodiment is after testing：Content of vanadium is 77.52 ~ 80.43wt%；Nitrogen content is
12.67~16.98wt%；Apparent density is 3.03 ~ 3.54g/cm3。
Therefore, present embodiment has the characteristics of technique is simple, the reaction time is short low with reaction temperature.
Claims (3)
1. a kind of preparation method of VN alloy, it is characterised in that be the step of the preparation method：
Step 1: being (0.1 ~ 0.3): 1 dispensing in mass ratio by carbonaceous reducing agent and the vanadic sulfate in terms of anhydride, mix,
Obtain mixed material；
Step 2: it is lump material by mixed material machine pressure, the density of the lump material is 1.5 ~ 2.0g/cm3；Again will
The lump material dries 1 ~ 7h under the conditions of 60 ~ 120 DEG C；
Step 3: under conditions of normal pressure and nitrogen flow are 100 ~ 600mL/min, dried lump material is heated to
1000 ~ 1400 DEG C, 1 ~ 5h is incubated, room temperature ~ 100 DEG C is cooled to the furnace, comes out of the stove, obtain VN alloy.
2. the preparation method of VN alloy according to claim 1, it is characterised in that the carbonaceous reducing agent is carbon black, stone
One or more of ink and activated carbon；The granularity of carbonaceous reducing agent is 0.074 ~ 0.250mm.
3. the preparation method of VN alloy according to claim 1, it is characterised in that the granularity of the vanadic sulfate is
0.074~0.250mm。
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| CN113718120B (en) * | 2021-08-22 | 2022-06-14 | 湖南众鑫新材料科技股份有限公司 | Process for synthesizing vanadium nitride from nitrogen and vanadium |
| CN114394578A (en) * | 2021-12-06 | 2022-04-26 | 武汉科技大学 | Vanadium nitride precursor and preparation method thereof |
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| AT329100B (en) * | 1970-09-09 | 1976-04-26 | Hollandse Metallurg Ind Billit | PROCESS FOR THE MANUFACTURING OF AN ADDITIVE TO STEEL |
| CN102173395A (en) * | 2011-01-05 | 2011-09-07 | 武安市炜荣物资有限公司 | Simple vanadium nitride production method |
| CN102936678A (en) * | 2012-12-03 | 2013-02-20 | 张春雨 | Vanadium-nitrogen alloy production method |
| CN103952512A (en) * | 2014-05-12 | 2014-07-30 | 徐春霞 | Method for preparing vanadium-nitrogen alloy |
| CN104016314A (en) * | 2014-06-26 | 2014-09-03 | 济南顺源新材料科技有限公司 | Preparation method of vanadium nitride |
| CN105483507A (en) * | 2016-01-05 | 2016-04-13 | 北京科技大学 | Nitrided ferrovanadium alloy and preparing method thereof |
| CN105838970A (en) * | 2016-04-15 | 2016-08-10 | 河北钢铁股份有限公司承德分公司 | Preparation method of high-nitrogen vanadium nitride |
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- 2016-12-01 CN CN201611091160.7A patent/CN106498266B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AT329100B (en) * | 1970-09-09 | 1976-04-26 | Hollandse Metallurg Ind Billit | PROCESS FOR THE MANUFACTURING OF AN ADDITIVE TO STEEL |
| CN102173395A (en) * | 2011-01-05 | 2011-09-07 | 武安市炜荣物资有限公司 | Simple vanadium nitride production method |
| CN102936678A (en) * | 2012-12-03 | 2013-02-20 | 张春雨 | Vanadium-nitrogen alloy production method |
| CN103952512A (en) * | 2014-05-12 | 2014-07-30 | 徐春霞 | Method for preparing vanadium-nitrogen alloy |
| CN104016314A (en) * | 2014-06-26 | 2014-09-03 | 济南顺源新材料科技有限公司 | Preparation method of vanadium nitride |
| CN105483507A (en) * | 2016-01-05 | 2016-04-13 | 北京科技大学 | Nitrided ferrovanadium alloy and preparing method thereof |
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