CN106222472A - A kind of low-carbon high-nitrogen vanadium-nitrogen alloy preparation method - Google Patents
A kind of low-carbon high-nitrogen vanadium-nitrogen alloy preparation method Download PDFInfo
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- CN106222472A CN106222472A CN201610553287.XA CN201610553287A CN106222472A CN 106222472 A CN106222472 A CN 106222472A CN 201610553287 A CN201610553287 A CN 201610553287A CN 106222472 A CN106222472 A CN 106222472A
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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
Abstract
The invention discloses the preparation method of a kind of low-carbon high-nitrogen VN alloy, the method uses to by containing barium oxide, carburization agent, catalyst, binding agent, nitridation accelerator and make blank, to blank heating, make the gasification of nitridation accelerator or decompose generation gas, crisscross Micro porosity or passage is formed in blank, nitrogen in nitridation reaction enters into internal participation of blank by these holes or passage and reacts, and makes nitridation reaction more complete, and nitrogen content is significantly increased；The present invention starts with from the carbonization of VN alloy, nitridation mechanism, by adding nitridation accelerator in dispensing, solve accelerated carbonation, a difficult problem for strengthening nitridation, compared with prior art, significantly improve the nitrogen content of VN alloy, reduce comprehensive production cost and the energy consumption of VN alloy；Moreover, change dress base operation, it is simple to the release of gas and the process of entrance, improve reaction effect.
Description
Technical field
The invention belongs to technical field of ferrous metallurgy, the low-carbon high-nitrogen vanadium nitrogen relating to adding in a kind of steelmaking process closes
The preparation method of gold.
Background technology
The vanadium of 80%-90% is used for steel and iron industry, and its main cause is the same carbon of vanadium, nitrogen reaction the formation carbon of infusibility, nitridation
Thing, these compounds can play precipitation-hardening and the effect of crystal grain refinement in steel.Therefore, vanadium carbide, the vanadium nitrogen of vanadium nitride composition
Alloy plays increasingly important effect in V-alloyed steel produces.VN alloy can be used for structural steel, tool steel, pipe line steel, reinforcing bar,
In ordinary skill steel and cast iron.Existing research shows: VN alloy makes an addition to improve in steel the wearability of steel, corrosion-resistant
Property, toughness, intensity, ductility and the comprehensive mechanical performance such as hardness and thermal fatigue resistance, and it is good solderable to make steel have
Performance, and the effects such as elimination field trash extension can be played.VN alloy and use is directly added in Hi-Stren steel
Vanadium iron is compared and is had the following advantages: more effectively play precipitation strength and crystal grain thinning than vanadium iron；Reduce the addition cost～40% of vanadium；
Be conducive to vanadium and the comprehensive utilization of nitrogen, significantly improve the comprehensive mechanical performance of steel.VN alloy reinforcement ratio regular reinforcement is used
Amount reduces about 14%.VN alloy is widely used in non-hardened and tempered steel and CSP high-intensity band steel,
And VN alloyization combines with TMCP technique and is applied in China's High Strength H-Beam produces.
At present, the mode that VN alloy uses barium oxide to add graphite reduction nitridation mostly produces, and uses this kind of mode raw
It is relatively big that the VN alloy produced also exists product quality fluctuation, and technique instability causes carbon content too high.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of low-carbon high-nitrogen VN alloy, on the basis of prior art
On, study from the process of nitridation reaction, solve discharging and the entrance problem participating in reacting gas of generated reactive gas, and
By strengthening the dynamic conditions of carbonization, nitridation in dispensing with addition of nitridation accelerator, promote carburizing reagent and nitridation reaction,
It is finally reached the nitrogen content improving VN alloy, obtains the nitrogenous stable and purpose of the higher vanadium-nitrogen alloy product of nitrogen content.
The technical solution used in the present invention is:
The preparation method of a kind of low-carbon high-nitrogen VN alloy, it is characterised in that comprise the steps of
S1 raw mill
To contain barium oxide uses Raymond mill to grind to form the powder that fineness is 100 ~ 200 mesh, uses Raymond mill to grind in graphite
The powder becoming fineness to be 30 ~ 60 mesh；
S2 dispensing mixes
According to containing barium oxide: bonding agent: catalyst: carburization agent: nitrogen fixation agent: nitridation accelerator=100:0.5 ~ 2:0.5 ~ 1.5:
Above-mentioned raw materials is joined in blender by the weight ratio of 25 ~ 35:0.5 ~ 2:0.5 ~ 1, is stirred mixing, is uniformly mixed
Compound, 70 ~ 80 ° of dried 12h are standby；
S3 pressed compact is aged
Use blank machine that the compound obtained in previous step is pressed into oblate blank, be subsequently placed in the shady and cool environment of ventilation
In carry out ripening, digestion time 7d；
S4 fills base
Uniformly being placed on by blank in previous step in food steamer structure graphite crucible, the gap between upper and lower two-layer blank is
3 ~ 5cm, is 1 ~ 3cm with the gap between adjacent two blank of layer；
S5 fires
Calcining kiln put into by the graphite crucible that will be equipped with blank, is first warming up to 200 ~ 300 DEG C, is incubated 10 ~ 12h, then to calcining
It is passed through nitrogen in kiln, keeps the air pressure in calcining kiln to control at 0.1 ~ 0.5MPa, be warming up to 650 ~ 660 DEG C, be incubated 4 ~ 5h, then
It is continuously heating to 1200 ~ 1250 DEG C, is incubated 4 ~ 5h；
S6 cooling down
Stopping heating, continue to be passed through nitrogen in calcining kiln, after naturally cooling to less than 100 DEG C, removal calcining kiln obtains vanadium nitrogen
Alloy.
Further, described is Vanadium sesquioxide, vanadium tetraoxide, vanadic anhydride and metavanadic acid containing barium oxide
One or more mixture in ammonium, ammonium poly-vanadate.
Further, described is vanadic anhydride containing barium oxide.
Further, described bonding agent is for the one in flour, tapioca starch, spent pulping liquor, syrup, polyvinyl alcohol or many
Plant mixture.
Further, one or more mixture during described catalyst is brown iron oxide, iron powder, vanadium iron powder, vanadium powder.
Further, described carburization agent is made up of electrode graphite, crystalline flake graphite and white carbon black, wherein, and the weight of electrode graphite
Amount percentage ratio is 30 ~ 60%, and the percentage by weight of crystalline flake graphite is 20 ~ 40%, and the percentage by weight of white carbon black is 10 ~ 30%.
Further, one or more mixture during described nitrogen fixation agent is calcium fluoride, calcium carbonate, calcium chloride.
Further, described nitridation accelerator be ammonium sulfate, ammonium hydrogen sulfate, ammonium carbonate, ammonium hydrogen carbonate, ammonium nitrate, chlorine
Change ammonium, ammonium poly-vanadate, ammonium metavanadate；One or more mixture in heavy oil, light oil, ferrous carbonate, at 500 DEG C, nitridation
Accelerator is heated and is decomposed, passage crisscross on blank or hole, and these passages are lived or hole becomes follow-up gas
The path of body turnover.
Further, the base of the column type that the graphite crucible used in described step S4 is closed by bottom surface and several ends
The pallet composition of the column type of face closure, has some passages, at described base side wall top on described base and pallet
And the top of pallet side wall and bottom are provided with the step of cooperation and make pallet can overlay on base, described base and pallet
The degree of depth be 5 ~ 10cm so that dress base simple and quick, blank is neat and orderly, it is simple to gas discharge and enter.
Further, it is some be placed in crucible body that the graphite crucible used in described step S4 has crucible body
Individual dividing plate and have in crucible body and dividing plate beginning several passages, be provided with below the edge of described dividing plate and uniformly set
The height having several bracers and a bracer is 5 ~ 10cm so that dress base is simple and quick, and blank is neat and orderly, just
In gas discharge and entrance.
The invention has the beneficial effects as follows:
Compared with prior art, by adding nitridation accelerator in dispensing, improve and enhance the kinetics bar of carbonization, nitridation
Part, solves and produces, by existing method, the problem that nitrogen-containing alloy nitrogen content is low and unstable；Nitridation accelerator is used to have making
Simply, the advantage such as cheap；Preparation cost and the energy consumption of the present invention are the lowest, can realize the rule of the nitrogen-containing alloy of high nitrogen content
Modelling is produced, and meets the market needs to high nitrogen content product.Meanwhile, dress base process in the present invention, compared to traditional icepro
Huddling and put, blank arrangement in the present invention in order, utilizes gaseous volatilization in blank, and blank is wrapped up by nitrogen, beneficially nitridation reaction
Process.
Accompanying drawing explanation
Fig. 1 is present invention process schematic flow sheet.
Fig. 2 is graphite crucible assembling structural representation in the present invention.
Fig. 3 is another structural representation of graphite crucible in invention.
Detailed description of the invention
In order to the advantage making the purpose of the present invention and technical scheme is clearer, below in conjunction with accompanying drawing and example, right
The present invention is further elaborated.
Shown in accompanying drawing 1, the preparation method of a kind of low-carbon high-nitrogen VN alloy, comprise the steps of
S1 raw mill
To contain barium oxide uses Raymond mill to grind to form the powder that fineness is 100 ~ 200 mesh, uses Raymond mill to grind in graphite
The powder becoming fineness to be 30 ~ 60 mesh；
S2 dispensing mixes
According to containing barium oxide: bonding agent: catalyst: carburization agent: nitrogen fixation agent: nitridation accelerator=100:0.5 ~ 2:0.5 ~ 1.5:
Above-mentioned raw materials is joined in blender by the weight ratio of 25 ~ 35:0.5 ~ 2:0.5 ~ 1, is stirred mixing, is uniformly mixed
Compound, 70 ~ 80 ° of dried 12h are standby；
S3 pressed compact is aged
Use blank machine that the compound obtained in previous step is pressed into oblate blank, be subsequently placed in the shady and cool environment of ventilation
In carry out ripening, digestion time 7d；
S4 fills base
Uniformly being placed on by blank in previous step in food steamer structure graphite crucible, the gap between upper and lower two-layer blank is
3 ~ 5cm, is 1 ~ 3cm with the gap between adjacent two blank of layer；
S5 fires
Calcining kiln put into by the graphite crucible that will be equipped with blank, is first warming up to 200 ~ 300 DEG C, is incubated 10 ~ 12h, then to calcining
It is passed through nitrogen in kiln, keeps the air pressure in calcining kiln to control at 0.1 ~ 0.5MPa, be warming up to 650 ~ 660 DEG C, be incubated 4 ~ 5h, then
It is continuously heating to 1200 ~ 1250 DEG C, is incubated 4 ~ 5h；
S6 cooling down
Stopping heating, continue to be passed through nitrogen in calcining kiln, after naturally cooling to less than 100 DEG C, removal calcining kiln obtains vanadium nitrogen
Alloy.
As shown in Figure 2, the base of column type that the graphite crucible used in described step S4 is closed by bottom surface and some
The pallet 2 of the column type that individual bottom surface is closed forms, and has some passages 3, at described base 1 on described base 1 and pallet 2
Top side wall and the top of pallet 2 sidewall and bottom are provided with the step 4 of cooperation and make pallet 2 can overlay on base 1, institute
The degree of depth stating base 1 and pallet 2 is 5 ~ 10cm.
Graphite crucible can also use another kind of structure.As shown in Figure 3, the graphite crucible used in described step S4 has
Crucible body 5 and several dividing plates 6 being placed in crucible body 5 and have in crucible body 5 and dividing plate 6 beginning several
Passage 3, being provided with below the edge of described dividing plate 6 and being uniformly provided with the height of several bracers 7 and bracer is 5 ~ 10cm.
Embodiment one
The raw material used is vanadic anhydride 100kg, polyvinyl alcohol 0.5kg, iron powder 0.5kg, electrode graphite 15kg, crystalline flake graphite
2.5kg, white carbon black 7.5kg, calcium fluoride 0.5kg, ammonium sulfate 0.5kg, VN alloy nitrogen content 15.5%, carbon content 5.1%.
Embodiment two
The raw material used is ammonium metavanadate 100kg, flour 2kg, brown iron oxide 1.5kg, electrode graphite 10.5kg, crystalline flake graphite
14kg, white carbon black 10.5kg, calcium chloride 2kg, ammonium carbonate 15kg, VN alloy nitrogen content 15.7%, carbon content 4.8%.
Embodiment three
The raw material used is vanadic anhydride 50kg, ammonium poly-vanadate 50kg, polyvinyl alcohol 1.5kg, iron powder 1.2kg, electrode graphite
9kg, crystalline flake graphite 12kg, white carbon black 9kg, calcium fluoride 1.3kg, ammonium sulfate 0.8kg, VN alloy nitrogen content 16.0%, carbon content
4.9%。
Claims (10)
1. the preparation method of a low-carbon high-nitrogen VN alloy, it is characterised in that comprise the steps of
S1 raw mill
To contain barium oxide uses Raymond mill to grind to form the powder that fineness is 100 ~ 200 mesh, uses Raymond mill to grind in graphite
The powder becoming fineness to be 30 ~ 60 mesh；
S2 dispensing mixes
According to containing barium oxide: bonding agent: catalyst: carburization agent: nitrogen fixation agent: nitridation accelerator=100:0.5 ~ 2:0.5 ~ 1.5:
Above-mentioned raw materials is joined in blender by the weight ratio of 25 ~ 35:0.5 ~ 2:0.5 ~ 1, is stirred mixing, is uniformly mixed
Compound, 70 ~ 80 ° of dried 12h are standby；
S3 pressed compact is aged
Use blank machine that the compound obtained in previous step is pressed into oblate blank, be subsequently placed in the shady and cool environment of ventilation
In carry out ripening, digestion time 7d；
S4 fills base
Uniformly being placed on by blank in previous step in food steamer structure graphite crucible, the gap between upper and lower two-layer blank is
3 ~ 5cm, is 1 ~ 3cm with the gap between adjacent two blank of layer；
S5 fires
Calcining kiln put into by the graphite crucible that will be equipped with blank, is first warming up to 200 ~ 300 DEG C, is incubated 10 ~ 12h, then to calcining
It is passed through nitrogen in kiln, keeps the air pressure in calcining kiln to control at 0.1 ~ 0.5MPa, be warming up to 650 ~ 660 DEG C, be incubated 4 ~ 5h, then
It is continuously heating to 1200 ~ 1250 DEG C, is incubated 4 ~ 5h；
S6 cooling down
Stopping heating, continue to be passed through nitrogen in calcining kiln, after naturally cooling to less than 100 DEG C, removal calcining kiln obtains vanadium nitrogen
Alloy.
The preparation method of a kind of low-carbon high-nitrogen VN alloy the most according to claim 1, it is characterised in that: described containing vanadium oxygen
Compound is one or more mixing in Vanadium sesquioxide, vanadium tetraoxide, vanadic anhydride and ammonium metavanadate, ammonium poly-vanadate
Thing.
The preparation method of a kind of low-carbon high-nitrogen VN alloy the most according to claim 2, it is characterised in that: described containing vanadium oxygen
Compound is vanadic anhydride.
The preparation method of a kind of low-carbon high-nitrogen VN alloy the most according to claim 1, it is characterised in that: described bonding agent
For for one or more mixture in flour, tapioca starch, spent pulping liquor, syrup, polyvinyl alcohol.
The preparation method of a kind of low-carbon high-nitrogen VN alloy the most according to claim 1, its spy is: described catalyst is
One or more mixture in brown iron oxide, iron powder, vanadium iron powder, vanadium powder.
The preparation method of a kind of low-carbon high-nitrogen VN alloy the most according to claim 1, it is characterised in that: described carbonization
Agent is made up of electrode graphite, crystalline flake graphite and white carbon black, and wherein, the percentage by weight of electrode graphite is 30 ~ 60%, crystalline flake graphite
Percentage by weight is 20 ~ 40%, and the percentage by weight of white carbon black is 10 ~ 30%.
The preparation method of a kind of low-carbon high-nitrogen VN alloy the most according to claim 1, it is characterised in that: described nitrogen fixation agent
For one or more mixture in calcium fluoride, calcium carbonate, calcium chloride.
The preparation method of a kind of low-carbon high-nitrogen VN alloy the most according to claim 1, it is characterised in that: described nitridation promotees
Enter agent for ammonium sulfate, ammonium hydrogen sulfate, ammonium carbonate, ammonium hydrogen carbonate, ammonium nitrate, ammonium chloride, ammonium poly-vanadate, ammonium metavanadate；Heavy oil,
One or more mixture in light oil, ferrous carbonate.
The preparation method of a kind of low-carbon high-nitrogen VN alloy the most according to claim 1, it is characterised in that: described step S4
The pallet (2) of the column type that the base (1) of the column type that the graphite crucible of middle employing is closed by bottom surface and several bottom surfaces are closed
Composition, has some passages (3), at described base (1) top side wall and pallet on described base (1) and pallet (2)
(2) top of sidewall and bottom are provided with the step (4) of cooperation and make pallet (2) can overlay on base (1), described base
And the degree of depth of pallet (2) is 5 ~ 10cm (1).
The preparation method of a kind of low-carbon high-nitrogen VN alloy the most according to claim 1, it is characterised in that: described step
The graphite crucible used in S4 has crucible body (5) and several dividing plates (6) being placed in crucible body (5) and in crucible basis
Have several passages of beginning (3) on body (5) and dividing plate (6), at described dividing plate (6) if edge below be provided with and be uniformly provided with
The height of a dry bracer (7) and a bracer is 5 ~ 10cm.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107699779A (en) * | 2017-08-29 | 2018-02-16 | 湖北华祥合金有限公司 | A kind of VN alloy and its production method |
| CN113621848A (en) * | 2021-08-05 | 2021-11-09 | 陕西中钒昌盛新材料科技有限公司 | Preparation method of high-nitrogen vanadium-nitrogen alloy |
| CN113737041A (en) * | 2021-08-27 | 2021-12-03 | 湖南众鑫新材料科技股份有限公司 | Method for industrial production of vanadium-nitrogen alloy product |
| CN114231781A (en) * | 2021-11-12 | 2022-03-25 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method of high-nitrogen vanadium-nitrogen alloy |
| CN115786760A (en) * | 2022-12-13 | 2023-03-14 | 攀钢集团钒钛资源股份有限公司 | Preparation method of high-density vanadium-nitrogen alloy material ball |
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| CN101603132A (en) * | 2009-07-16 | 2009-12-16 | 钢铁研究总院 | A kind of method and apparatus of production VN alloy |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107699779A (en) * | 2017-08-29 | 2018-02-16 | 湖北华祥合金有限公司 | A kind of VN alloy and its production method |
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| CN113737041A (en) * | 2021-08-27 | 2021-12-03 | 湖南众鑫新材料科技股份有限公司 | Method for industrial production of vanadium-nitrogen alloy product |
| CN114231781A (en) * | 2021-11-12 | 2022-03-25 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method of high-nitrogen vanadium-nitrogen alloy |
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| CN115786760A (en) * | 2022-12-13 | 2023-03-14 | 攀钢集团钒钛资源股份有限公司 | Preparation method of high-density vanadium-nitrogen alloy material ball |
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Application publication date: 20161214 |