CN106498266A - A kind of preparation method of VN alloy - Google Patents
A kind of preparation method of VN alloy Download PDFInfo
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- CN106498266A CN106498266A CN201611091160.7A CN201611091160A CN106498266A CN 106498266 A CN106498266 A CN 106498266A CN 201611091160 A CN201611091160 A CN 201611091160A CN 106498266 A CN106498266 A CN 106498266A
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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：The vanadium oxysulfate that counts by carbonaceous reducing agent and with anhydride is in mass ratio as (0.1 ~ 0.3): 1 dispensing, mixes, obtains 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 under the conditions of 60 ~ 120 DEG C 1 ~ 7h again.Under conditions of normal pressure and nitrogen flow are 100 ~ 600mL/min, dried lump material are heated to 1000 ~ 1400 DEG C, 1 ~ 5h are incubated, are cooled 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 vanadium oxysulfate is 0.074 ~ 0.250mm.The characteristics of present invention has process is simple, short response time and low reaction temperature.
Description
Technical field
The invention belongs to vanadium alloy technical field.Specifically related to a kind of preparation method of VN alloy.
Background technology
VN alloy is a kind of new alloy addition, makes an addition in steel and can be carried by precipitation strength and refined crystalline strengthening
The comprehensive mechanical performances such as the intensity of Gao Gang, toughness, ductility, wearability, corrosion resistance and thermal fatigue resistance, can be effectively improved
The welding performance of steel.Compared with vanadium iron is added 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, and the effectively save rolled steel dosage of energy can economize in raw materials and smelting cost, with huge
Resources conservation and environmental conservation double benefit.
The preparation method of traditional VN alloy is by vanadic anhydride, vanadium tetraoxide, Vanadium sesquioxide, metavanadic acid
Ammonium, ammonium poly-vanadate etc., are generated with nitrogen or ammonia reaction with addition of reducing agent, binding agent, accelerator etc. at high temperature as raw material
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, pressure ball after wet mixing is added to dry, in 800 DEG C of prereduction 5h or so, be warming up to 1350 after mixing
DEG C persistently the drastic reduction more than 6h and carbonization, are constantly filled with more than 99.99% nitrogen in 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, completes in 20h or so, reaction total time, cooled down
Come out of the stove to 150 DEG C, VN alloy is obtained.
" a kind of method for preparing VN alloy "（CN103952512A）Patented technology, by ammonium metavanadate or/and many vanadic acid
Ammonium reduces 3 ~ 6h in 600 ~ 650 DEG C under nitrogen and hydrogen mixture atmosphere, obtains barium oxide；By the barium oxide for obtaining and catalyst,
Carbonaceous powder, binding agent and water wet method ball, are incubated 1 ~ 3h in 300 ~ 350 DEG C under normal pressure blanket of nitrogen, then heat to 1450 ~
1650 DEG C, nitrogen of the charged pressure for positive 0.04 ~ 0.08MPa carries out 6 ~ 9h of nitridation reaction, and cooling discharge obtains VN alloy.
" a kind of vanadium nitrogen alloy preparation method "（CN102936678A）Patented technology, will contain vanadium raw materials powder, iron powder, carbonaceous powders
Agent and binding agent stirring mixing after compound stalk forming, then with rice husk by volume 1: 1 ratio send into calcining kiln, under oxygen free condition do
Process is evaporated, temperature is 600 ~ 650 DEG C, and the time is 6 ~ 7h, is then heated to 1300 ~ 1500 DEG C, while high pure nitrogen is passed through, the time
2 ~ 4h, cooling come out of the stove and obtain 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 length and preparation temperature are high.
Content of the invention
It is contemplated that overcoming prior art defect, it is therefore an objective to provide a kind of process is simple, the response time is short and reaction is warm
The preparation method of the low VN alloy of degree.
For achieving the above object, the technical solution used in the present invention is comprised the concrete steps that：
Step one, the vanadium oxysulfate that counts by carbonaceous reducing agent and with anhydride are in mass ratio as (0.1 ~ 0.3): 1 dispensing, 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；
The lump material is dried under the conditions of 60 ~ 120 DEG C 1 ~ 7h 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, is come 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 vanadium oxysulfate is 0.074 ~ 0.250mm.
Due to adopting above-mentioned technical proposal, the invention has the beneficial effects as follows：
(1) present invention adopts vanadium oxysulfate as raw material, as vanadium oxysulfate contains water of crystallization and absorption water, during agglomeration
Without the need for outer adding additives, process is simple.
(2) vanadium oxysulfate that the present invention is adopted decomposes in heating process so that the specific surface area increase of material, increased
With the contact area of nitrogen, reduction nitridation speed is improve, nitrogen content is increased, without the need for added promoter and the reduction nitridation time
Short.
(3) reaction temperature of the present invention is low, is conducive to energy efficient.
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 characteristics of present invention has process is simple, short response time and low reaction temperature.
Specific 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 that states.
Embodiment 1
A kind of preparation method of VN alloy.The technical scheme that the present embodiment is adopted is comprised the concrete steps that：
Step one, the vanadium oxysulfate that counts by carbonaceous reducing agent and with anhydride are in mass ratio as (0.1 ~ 0.2): 1 dispensing, mix,
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 under the conditions of 60 ~ 120 DEG C 1 ~ 7h 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, is come 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 vanadium oxysulfate 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 with 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 is adopted is comprised the concrete steps that：
Step one, the vanadium oxysulfate that counts by carbonaceous reducing agent and with anhydride are in mass ratio as (0.2 ~ 0.3): 1 dispensing, mix,
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 under the conditions of 60 ~ 120 DEG C 1 ~ 7h 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, is come 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 vanadium oxysulfate 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 with 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 is adopted is comprised the concrete steps that：
Step one, the vanadium oxysulfate that counts by carbonaceous reducing agent and with anhydride are in mass ratio as (0.15 ~ 0.25): 1 dispensing, mix
Even, 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 under the conditions of 60 ~ 120 DEG C 1 ~ 7h 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, is come 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 vanadium oxysulfate 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 with 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 with 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 this specific embodiment is：
(1) this specific embodiment, is being made using vanadium oxysulfate as raw material as vanadium oxysulfate contains water of crystallization and absorption water
Without the need for outer adding additives during block, process is simple.
(2) vanadium oxysulfate that this specific embodiment is adopted decomposes in heating process so that the specific surface area of material increases
Greatly, the contact area with nitrogen is increased, reduction nitridation speed is improve, be increased nitrogen content, without the need for added promoter and also
Former nitridation time is short.
(3) this specific embodiment reaction temperature is low, is conducive to energy efficient.
VN alloy prepared by this specific 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, the characteristics of this specific embodiment has short process is simple, response time and low reaction temperature.
Claims (3)
1. a kind of preparation method of VN alloy, it is characterised in that the step of the preparation method be：
Step one, the vanadium oxysulfate that counts by carbonaceous reducing agent and with anhydride are in mass ratio as (0.1 ~ 0.3): 1 dispensing, 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, is come 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 vanadium oxysulfate is
0.074~0.250mm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113718120A (en) * | 2021-08-22 | 2021-11-30 | 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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| 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 |
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| 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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| AT329100B (en) * | 1970-09-09 | 1976-04-26 | Hollandse Metallurg Ind Billit | PROCESS FOR THE MANUFACTURING OF AN ADDITIVE TO STEEL |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113718120A (en) * | 2021-08-22 | 2021-11-30 | 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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