CN104404333A - Raw material composition for preparing vanadium nitride with ultrahigh nitrogen content and method utilizing same to prepare ultrahigh vanadium nitride - Google Patents
Raw material composition for preparing vanadium nitride with ultrahigh nitrogen content and method utilizing same to prepare ultrahigh vanadium nitride Download PDFInfo
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- CN104404333A CN104404333A CN201410630205.8A CN201410630205A CN104404333A CN 104404333 A CN104404333 A CN 104404333A CN 201410630205 A CN201410630205 A CN 201410630205A CN 104404333 A CN104404333 A CN 104404333A
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Abstract
The invention relates to the field of steel metallurgy, and especially relates to a raw material composition for preparing vanadium nitride with an ultrahigh nitrogen content and a method utilizing the same to prepare ultrahigh vanadium nitride. The composition comprises a vanadium-containing compound, a carbonaceous reducing agent, and an adhesive; wherein the adhesive is melamine. The provided composition and method can achieve low-cost massive production of VN19 alloy product. The produced vanadium nitride with an ultrahigh nitrogen content has been applied to high strength thread steel production experiments in the Panzhihua steel group. The product quality indexes are as follows: nitrogen content is 17-21%, carbon content is less than 2.0%, oxygen content is less than 2.0%, and vanadium content is 75 to 78%.
Description
Technical field
The present invention relates to field of steel metallurgy, particularly relate to a kind of feedstock composition for the preparation of superelevation vanadium nitride and adopt this raw material to prepare the method for superelevation vanadium nitride.
Background technology
Vanadium nitrogen 19 is the high-level products in VN alloy series product, belong to high added value vanadium deep processed product, the production of vanadium iron for microalloyed steel can be substituted, add the comprehensive mechanical performances such as intensity, toughness, ductility and the thermal fatigue resistance that can improve steel in steel, effectively improve the welding property of steel.Under same intensity, add alloy of vanadium nitride, vanadium add-on 30-40% can be saved, significantly reduce steel making working procedure cost.
Because output of steel sharply expands in recent years, section bar turnout increases, and casting and rolling process application is increasingly extensive, and roll speed and finish to gauge speed improve greatly, and wherein many are all the new grade III steels containing vanadium.Therefore, require to reduce the solubleness of vanadium carbide nitride in ferrite, improve its speed from ferrite Precipitation Temperature and precipitation, with the maximized effect utilizing vanadium to reach precipitation strength.
There are some researches show, in crystal, ferritic formation mainly exists because there is vanadium nitride to precipitate in austenite.Even if in the technique adopting vanadium iron, vanadium is all start to separate out inside austenite with the form of almost pure vanadium nitride, and the beginning temperature separated out sharply raises with the rising of nitrogen content, only when nitrogen is soon used up, just gradual change forms the isomorphous precipitation of vanadium carbide nitride.Under the size of precipitation strength effect from austenite to ferritic phase transition process and given transformation temperature, the dissolving power of vanadium carbide nitride is inversely proportional to.And the dissolving power of vanadium carbide in austenite is more much higher than vanadium nitride, pure vanadium carbide even can not produce precipitation inside austenite.In addition, for vanadium micro-alloyed steel, often increase the nitrogen of 10ppm, yield strength can be made to increase 6MPa, and this relation is almost linear.In sum, nitrogen takes on important role in precipitation strength.It plays an important role in the formation of vanadium carbide nitride promoting a large amount of and even dispersion in raising rolling temperature and speed etc., and making nitrogen become the effect of control precipitation strength becomes first-selected element with the yield strength aspect improving steel.
Chinese invention patent (application number: 200910194234.3 applyings date: 2009-11-27) discloses a kind of preparation method of vanadium nitride, and vanadium-containing compound mixes with organic nitrogen compound by this preparation method, calcines, obtain vanadium nitride in nitrogenous gas.
Chinese invention patent (application number: the 201210291750.X applying date: 2012-08-16) discloses a kind of preparation method of vanadium nitride, this preparation method is by powdery vanadium oxide compound, carbonaceous reducing agent and caking agent aqueous solution evenly after be pressed into bulk, join in two channels pushed bat kiln continuously after again lumpy material being dried, under kiln inner pressure 10-100Pa and gas protective condition, in kiln, each temperature province is reduced, sintering, nitrogenizing reaction and cooling, it is 77-80%V that final production goes out to obtain content, 11-18%N, 2-8%C, product density 3.2-4.1g/cm
3vanadium nitride product.The method achieve continuous seepage, have raw material and be easy to get, stable technical process, production efficiency is high, and reduction efficiency is high, and temperature of reaction is low, and thermo-efficiency is high, low power consumption and other advantages.
Chinese invention patent (application number: 201310614215.8 applyings date: 2013-11-28) discloses with powdery Vanadium Pentoxide in FLAKES and carbon black as raw material, powdery Vanadium Pentoxide in FLAKES and carbon black are mixed according to mass ratio 1 ︰ (0.33 ~ 0.35), the water of additional raw material 4 ~ 6wt% again, mixing, be pressed into autoreduction ball, autoreduction ball is loaded electrical heater, in nitrogen atmosphere, is warming up to 620 ~ 650 DEG C, is incubated 1.5 ~ 2.5 hours; Then be warming up to 1250 ~ 1300 DEG C, be incubated 2 ~ 3 hours, furnace cooling; Finally that the vanadium nitride after coming out of the stove is broken, after broken, the concentration of additional raw material 2 ~ 3wt% is the polyvinyl alcohol water solution of 4%, stirring and evenly mixing, with powerful ball press compacting balling-up, obtains alloy of vanadium nitride.The pressure of described compacting balling-up is 12 ~ 14MPa, repeats compacting 2 ~ 3 times.The method has the advantages that technique is simple, workable, with short production cycle, energy consumption is low and production cost is low, and prepared alloy of vanadium nitride stay in grade, nitrogen content is high and apparent density is higher.
Chinese invention patent (application number: 201410289772.1 applyings date: 2014-06-26) discloses and adopts the hot legal system of liquid phase solvent for vanadium nitride, liquid phase adopts the aqueous solution or alcoholic solvent, vanadium source is the divalence of vanadium, trivalent or tetravalence muriate, vitriol, nitrate and acetate, and nitrogenous source is ammonia, urea, hydrazine, ammonium chloride, volatile salt, ammonium acetate, ammonium sulfate.The method preparation process does not need to adopt carbon or hydrogen as reductive agent, and eliminate the discharge of preparation process percent of greenhouse gases, also eliminate the carbon impurity element in vanadium nitride simultaneously, the method interalloy synthesis temperature is lower than 400 DEG C; Present method synthesis vanadium nitride nitrogen content the highest can reach 21% theoretical content.
Chinese invention patent (application number: 201410309698.5 applyings date: 2014-07-01) discloses a kind of ferrovanadium nitride and preparation method thereof, the method comprises the following steps: barium oxide, carbonaceous powder, iron powder, aqueous binders and nitrogenize promotor are mixed mutually and compacting, forms material block; Carry out drying to material block, then block is expected in heating in a nitrogen atmosphere in the reactor, cooling after heating, thus obtains ferrovanadium nitride.The method, through reasonable batching and the exact operations to equipment, can significantly improve the apparent density of ferrovanadium nitride, and improves the nitrogen content in ferrovanadium nitride.
At present, vanadium nitrogen 19 is the high-level products in VN alloy series product, belong to high added value vanadium deep processed product, the production of vanadium iron for microalloyed steel can be substituted, add the comprehensive mechanical performances such as intensity, toughness, ductility and the thermal fatigue resistance that can improve steel in steel, effectively improve the welding property of steel.Under same intensity, add alloy of vanadium nitride, vanadium add-on 30-40% can be saved, significantly reduce steel making working procedure cost, at present, market sale is main mainly with vanadium nitrogen 16 alloy, is guaranteeing under vanadium nitrogen 16 alloy output and the prevailing prerequisite of sales volume, accelerates the new-product development dynamics of higher category, make full use of advanced shaft furnace production technique, adjustment formula and processing technology, repeatedly studies and production test, achieves the mass production of VN19 alloy product under low cost condition.
Summary of the invention
An object of the present invention is to provide a kind of feedstock composition for the preparation of superelevation vanadium nitride, adopt this feedstock composition to produce vanadium nitride, the nitrogen content in vanadium nitride is high, decreases the time required for nitrogenize, has saved energy consumption, extends the work-ing life of stove.Second object of the present invention is to provide the method adopting above-mentioned raw materials composition to prepare superelevation vanadium nitride.
In order to realize first above-mentioned object, present invention employs following technical scheme:
For the preparation of a feedstock composition for superelevation vanadium nitride, said composition comprises vanadium-containing compound, carbonaceous reducing agent and binding agent, and described binding agent is trimeric cyanamide.
As preferably, this feedstock composition is formed primarily of following composition by weight: vanadium-containing compound 100 parts, Powdered carbonaceous reducing agent 10 ~ 40 parts, trimeric cyanamide 1 ~ 15 part.
As preferred again, this feedstock composition is formed primarily of following composition by weight: vanadium-containing compound 100 parts, Powdered carbonaceous reducing agent 18 ~ 25 parts, trimeric cyanamide 3 ~ 8 parts.
As preferably, this feedstock composition also comprises the water of below feedstock composition 2% weight ratio.
As preferably, described vanadium-containing compound is at least one in ammonium meta-vanadate, poly ammonium vanadate, Vanadium Pentoxide in FLAKES, vanadium dioxide, vanadous oxide.
As preferred again, described vanadium-containing compound is Vanadium Pentoxide in FLAKES or vanadous oxide or both mixtures.
As preferably, described carbonaceous reducing agent is one or more in gac, carbon black, natural graphite, graphous graphite powder and crystalline flake graphite.
As preferred again, described carbonaceous reducing agent is Powdered graphous graphite powder, and granularity is 80 ~ 150 orders.
In order to realize second above-mentioned object, present invention employs following technical scheme:
A preparation method for superelevation vanadium nitride, the method comprises the following steps:
1) be pressed into after above-mentioned a kind of mixing of the feedstock composition for the preparation of superelevation vanadium nitride the work in-process ball that diameter is 30 ~ 60mm, more naturally dry;
2) the work in-process ball after drying being dropped into middle-end is continuously provided with in the shaft kiln of medium-frequency induction furnace, material is first through the upper end preheating and drying of shaft kiln, drying temperature is 400 ~ 600 DEG C, time is 1 ~ 2 hour, then the medium-frequency induction furnace of shaft kiln middle-end is arrived, medium-frequency induction furnace passes into high pure nitrogen, keep pressure-fired 0.01 ~ 0.03MPa in stove, temperature 900 ~ 1150 DEG C, carry out carbonization nitrogenizing reaction 4 ~ 6 hours, finally arrive shaft kiln lower end and carry out cooling 1 ~ 2 hour, be cooled to 150 DEG C with bottom discharge, fed intake once every 6 ~ 8 hours like this, discharging once.
As preferably, described medium-frequency induction furnace is the Medium frequency induction shaft furnace of heating collar diameter at 500mm-1000mm.
The present invention is owing to have employed above-mentioned technical scheme, adopt trimeric cyanamide as binding agent, the not residual any impurity of the decomposition of trimeric cyanamide in reaction process, decompose the nitrogen element produced and can be used as cryogenic nitrogen agent, decompose the protium produced and can be used as low-temperature reduction agent, the oxygen element content in vanadium oxide is obviously reduced; The hole that trimeric cyanamide is formed after decomposing makes the specific surface area of Low Valent Vanadium oxide compound improve greatly, this makes the contact area of high-temperature ammonolysis stage and nitrogen improve, and therefore the nitrogen content of vanadium nitride is high, decreases the time required for nitrogenize, save energy consumption, extend the work-ing life of stove.
The present invention achieves the mass production of VN19 alloy product under low cost condition.The vanadium nitride of the superelevation nitrogen content produced has carried out the production test of high-strength deformed steel bar climbing steel.Product quality indicator: nitrogen content: 17-21%, carbon content < 2.0%, oxygen level < 2.0%, content of vanadium 75-78%.
Embodiment
embodiment 1
Be the powdery Vanadium Pentoxide in FLAKES of 98% by 100kg purity, 22kg granularity is that after the trimeric cyanamide of 100 object Graphite Powder 99s and 6kg mixes, make the work in-process ball of diameter 50mm ± 0.5mm with high-pressure ball press, seasoning is for subsequent use after 3 ~ 5 days.When feeding intake, work in-process ball being dropped into middle-end is continuously provided with in the shaft kiln of medium-frequency induction furnace, and material is first through the upper end preheating and drying of shaft kiln, and drying temperature is 500 DEG C, and the time is 1 hour, and then arrive the medium-frequency induction furnace of shaft kiln middle-end, medium-frequency induction furnace is with 14m
3/ h passes into high pure nitrogen, keeps pressure-fired 0.02MPa in stove, temperature 1000 DEG C ± 100 DEG C, carry out carbonization nitrogenizing reaction 4 hours, finally arrive the storing cooling room of shaft kiln lower end, the water cooling of cooling room jacketed, cool 1 hour, be cooled to 150 DEG C with bottom discharge, fed intake once every 6 hours, once, charging upper end furnace body temperature is at 500 DEG C for the second time, continuous seepage in discharging, product V:75.96% can be obtained, N:18.54%, C:1.16%, density 3.5g/cm3.
embodiment 2
Be the powdery Vanadium Pentoxide in FLAKES of 98% by 100kg purity, 20kg granularity is 100 object Graphite Powder 99s, after the trimeric cyanamide of 6kg mixes, make the work in-process ball of diameter 50mm ± 0.5mm with high-pressure ball press, seasoning is for subsequent use after 3 ~ 5 days.When feeding intake, work in-process ball being dropped into middle-end is continuously provided with in the shaft kiln of medium-frequency induction furnace, and material is first through the upper end preheating and drying of shaft kiln, and drying temperature is 550 DEG C, and the time is 1 hour, and then arrive the medium-frequency induction furnace of shaft kiln middle-end, medium-frequency induction furnace is with 14m
3/ h passes into high pure nitrogen, keeps pressure-fired 0.02MPa in stove, temperature 1000 DEG C ± 100 DEG C, carry out carbonization nitrogenizing reaction 4 hours, finally arrive the storing cooling room of shaft kiln lower end, the water cooling of cooling room jacketed, cool 1 hour, be cooled to 150 DEG C with bottom discharge, fed intake once every 6 hours, once, charging upper end furnace body temperature is at 550 DEG C for the second time, continuous seepage in discharging, product V:77.17% can be obtained, N:19.29, %C:1.53, density 3.15g/cm3.
embodiment 3
Be the powdery Vanadium Pentoxide in FLAKES of 98% by 100kg purity, 24kg granularity is 100 object Graphite Powder 99s, after the trimeric cyanamide of 6kg mixes, make the work in-process ball of diameter 50mm ± 0.5mm with high-pressure ball press, seasoning is for subsequent use after 3 ~ 5 days.When feeding intake, work in-process ball being dropped into middle-end is continuously provided with in the shaft kiln of medium-frequency induction furnace, and material is first through the upper end preheating and drying of shaft kiln, and drying temperature is 450 DEG C, and the time is 1 hour, and then arrive the medium-frequency induction furnace of shaft kiln middle-end, medium-frequency induction furnace is with 14m
3/ h passes into high pure nitrogen, keeps pressure-fired 0.02MPa in stove, temperature 1000 DEG C ± 100 DEG C, carry out carbonization nitrogenizing reaction 4 hours, finally arrive the storing cooling room of shaft kiln lower end, the water cooling of cooling room jacketed, cool 1 hour, be cooled to 150 DEG C with bottom discharge, fed intake once every 6 hours, once, charging upper end furnace body temperature is at 450 DEG C for the second time, continuous seepage in discharging, product V:78.27% can be obtained, N:20.69, %C:1.06, density 3.1g/cm3.
Claims (10)
1. for the preparation of a feedstock composition for superelevation vanadium nitride, said composition comprises vanadium-containing compound, carbonaceous reducing agent and binding agent, it is characterized in that: described binding agent is trimeric cyanamide.
2. a kind of feedstock composition for the preparation of superelevation vanadium nitride according to claim 1, it is characterized in that this feedstock composition is formed primarily of following composition by weight: vanadium-containing compound 100 parts, Powdered carbonaceous reducing agent 10 ~ 40 parts, trimeric cyanamide 1 ~ 15 part.
3. a kind of feedstock composition for the preparation of superelevation vanadium nitride according to claim 1, it is characterized in that this feedstock composition is formed primarily of following composition by weight: vanadium-containing compound 100 parts, Powdered carbonaceous reducing agent 18 ~ 25 parts, trimeric cyanamide 3 ~ 8 parts.
4. a kind of feedstock composition for the preparation of superelevation vanadium nitride according to claim 1 ~ 3 any one claim, is characterized in that: this feedstock composition also comprises the water of below feedstock composition 2% weight ratio.
5. a kind of feedstock composition for the preparation of superelevation vanadium nitride according to claim 1 ~ 3 any one claim, is characterized in that: vanadium-containing compound is at least one in ammonium meta-vanadate, poly ammonium vanadate, Vanadium Pentoxide in FLAKES, vanadium dioxide, vanadous oxide.
6. a kind of feedstock composition for the preparation of superelevation vanadium nitride according to claim 5, is characterized in that: vanadium-containing compound is Vanadium Pentoxide in FLAKES or vanadous oxide or both mixtures.
7. a kind of feedstock composition for the preparation of superelevation vanadium nitride according to claim 1 ~ 3 any one claim, is characterized in that: carbonaceous reducing agent is one or more in gac, carbon black, natural graphite, graphous graphite powder and crystalline flake graphite.
8. a kind of feedstock composition for the preparation of superelevation vanadium nitride according to claim 7, it is characterized in that: carbonaceous reducing agent is Powdered graphous graphite powder, granularity is 80 ~ 150 orders.
9. a preparation method for superelevation vanadium nitride, is characterized in that the method comprises the following steps:
1) be pressed into after a kind of mixing of the feedstock composition for the preparation of superelevation vanadium nitride described in claim 1 ~ 8 any one the work in-process ball that diameter is 30 ~ 60mm, more naturally dry;
2) the work in-process ball after drying being dropped into middle-end is continuously provided with in the shaft kiln of medium-frequency induction furnace, material is first through the upper end preheating and drying of shaft kiln, drying temperature is 400 ~ 600 DEG C, time is 1 ~ 2 hour, then the medium-frequency induction furnace of shaft kiln middle-end is arrived, medium-frequency induction furnace passes into high pure nitrogen, keep pressure-fired 0.01 ~ 0.03MPa in stove, temperature 900 ~ 1150 DEG C, carry out carbonization nitrogenizing reaction 4 ~ 6 hours, finally arrive shaft kiln lower end and carry out cooling 1 ~ 2 hour, be cooled to 150 DEG C with bottom discharge, fed intake once every 6 ~ 8 hours like this, discharging once.
10. the preparation method of a kind of superelevation vanadium nitride according to claim 9, is characterized in that: medium-frequency induction furnace is the Medium frequency induction shaft furnace of heating collar diameter at 500mm-1000mm.
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CN105671393A (en) * | 2016-01-07 | 2016-06-15 | 湖北湖大天沭新能源材料工业研究设计院有限公司 | Preparation method for micro-negative-pressure vanadium nitride and product thereof |
CN107012385A (en) * | 2017-04-10 | 2017-08-04 | 攀钢集团研究院有限公司 | The preparation method of high nitrogen VN alloy |
CN110923558A (en) * | 2019-10-30 | 2020-03-27 | 中色(宁夏)东方集团有限公司 | Preparation method of high-nitrogen vanadium-nitrogen alloy |
CN114195522A (en) * | 2021-11-30 | 2022-03-18 | 松山湖材料实验室 | Method for rapidly preparing vanadium nitride ceramic powder by using urea nitridation, product and application thereof |
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CN105671393A (en) * | 2016-01-07 | 2016-06-15 | 湖北湖大天沭新能源材料工业研究设计院有限公司 | Preparation method for micro-negative-pressure vanadium nitride and product thereof |
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CN114195522A (en) * | 2021-11-30 | 2022-03-18 | 松山湖材料实验室 | Method for rapidly preparing vanadium nitride ceramic powder by using urea nitridation, product and application thereof |
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