CN104018056A - Preparation method of nitrided ferrovanadium with high quality and low cost - Google Patents
Preparation method of nitrided ferrovanadium with high quality and low cost Download PDFInfo
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Abstract
The invention discloses a preparation method of nitrided ferrovanadium with high quality and low cost. The method comprises the following steps: evenly mixing a vanadium-containing compound, a carbon-containing compound, a compound for increasing nitrogen, an accelerant and an adhesive with water in a stirring manner, pressing into balls for molding and drying so as to obtain ball block materials; and sending the ball block materials into a furnace, carrying out high-temperature calcination and a nitridation reaction on the ball blocks at a high temperature and high purity and under the protection of nitrogen atmospheres, cooling to reach a constant-temperature state and taking out of the furnace after the cooling and the like, thereby obtaining the nitrided ferrovanadium at final. According to the method, the materials put into the furnace can be sintered to form the nitrided ferrovanadium by one step after the materials are evenly mixed and molded, so that the process is simple, easy to implement, strong in operability and less in investment as well as realizes energy conservation and consumption reduction, thereby substantially improving the production capacity. The mixed materials comprise the compound for increasing nitrogen, so that the nitriding process can be simultaneously carried out in the ball block materials which are molded in a mixing manner, i.e., the nitriding process can be finished well without a high pressure condition. The optimal settings of the temperature, the time and other parameters during the sintering process are further carried out, so that the sintering process is simple; and the nitrided ferrovanadium is high in yield and ideal in quality.
Description
Technical field
The present invention relates to the production method of the alloy addition that Iron and Steel Production uses, relate to the preparation method's, particularly a kind of high-quality low-cost of ferrovanadium nitride ferrovanadium nitride preparation method.
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 products such as high strength spiral shell mosquito reinforcing bar, high-strength line-pipe steel, high strength shaped steel, CSP high-strength steel strip, non-hardened and tempered steel, rapid tool steel.A large amount of real application data show, reaching under the comprehensive mechanical performances such as same intensity, toughness, ductility and thermal fatigue resistance, than adding, the Mechanical Fluctuation value of other vanadium alloy steel is little, mechanical property minimum value is high, and makes steel have good solderability.Owing to adding the vanadium recovery high (can reach more than 95%) of ferrovanadium nitride technique, save vanadium 30-40% than adding other vanadium iron, save vanadium more than 10% than adding VN alloy, thereby reduced steel product cost, be therefore subject to user and extensively welcome.Add ferrovanadium nitride basic identical with straight carbon steel technique on smelting, continuous casting, rolling technology, therefore simple to operate, be easy to control, and can eliminate the strain aging phenomenon of steel.
Ferrovanadium nitride can reach 5.0g/cm because of its proportion
3above, than adding vanadium nitride (proportion 3.5g/cm
3left and right) there is higher specific absorption, the high 3-5% of average specific VN alloy specific absorption, performance is more stable, has higher crystal grain thinning and promotes the functions such as intensity, toughness, ductility.Show according to published data: desirable ferrovanadium nitride V/N value is 3.64.
The preparation method of traditional ferrovanadium nitride mainly contains liquid nitriding process and solid State Nitriding method.Liquid nitriding, is that the qualified vanadium iron melt of smelting in electric furnace is put into the ladle of being with the hole brick of knowing how things stand and feel confident, passes into nitrogen simultaneously and carries out liquid nitriding, makes ferrovanadium nitride.Solid State Nitriding, is that vanadium iron powder is carried out to solid State Nitriding, makes ferrovanadium nitride.But be no matter that liquid nitriding or solid State Nitriding method are produced ferrovanadium nitride, first all will first produce ferro-vanadium, then vanadium iron could be carried out to nitriding treatment, and nitriding process need just can carry out under condition of high voltage, energy consumption does not meet greatly economic benefit.There are the following problems for the preparation method of above traditional ferrovanadium nitride: vanadium recovery is low, and nitrogen content is low, and production process complexity consumes energy high, and equipment investment cost is high.
In order to improve traditional preparation method or to grope new preparation method, people have done a lot of technological improvements, are below the example of prior art:
Example 1: publication number is CN102477511A, in the Chinese patent of " a kind of preparation method of ferrovanadium nitride " by name, a kind of preparation method of ferrovanadium nitride is disclosed, the method comprises: ferrovanadium dust is heated under nitrogen atmosphere, then carry out cooling, it is characterized in that, heat-processed comprises pre-heating stage, transitory stage and nitridation sintered stage, and the Heating temperature of described pre-heating stage be 400 DEG C to lower than 800 DEG C, the Heating temperature of described transitory stage be 800 DEG C to lower than 1200 DEG C, the Heating temperature in described nitridation sintered stage is 1200-1500 DEG C.The ferrovanadium nitride of described preparation has higher nitrogen content and apparent density.
Example 2: publication number is CN102976290A, in the Chinese patent of " a kind of preparation method of ferrovanadium nitride " by name, the preparation method who discloses another kind of ferrovanadium nitride, comprises the following steps: A: vanadium-containing compound, solid reductant, reduced iron powder are uniformly mixed into type; B: steps A gained material is put into the reactor under nitrogen protection atmosphere reacts 6-10 hour under 1300-1600 DEG C of high temperature; C: step B products therefrom migrates out cooling, obtains ferrovanadium nitride product when 120 DEG C of temperature <.It is simple for process, workable, energy-saving and cost-reducing, invests lessly, can significantly improve the throughput of vanadium-nitrogen alloy product.
Adopt the ferrovanadium nitride preparation method of above technology certainly can use, but have the following disadvantages:
Example 1 is real is the improvement way on conventional approach basis.First still to first produce ferro-vanadium, then vanadium iron could be carried out to nitriding treatment.Though nitrogen content improves, vanadium recovery is still low, and production process is still complicated, and energy consumption is still high, and equipment investment cost is still higher.
Though example 2 does not need first to produce ferro-vanadium; vanadium-containing compound, solid reductant, reduced iron powder to be uniformly mixed into the reactor sintering of putting under nitrogen protection atmosphere after type generate ferrovanadium nitride; simple for process; workable; energy-saving and cost-reducing; invest lessly, can significantly improve the throughput of vanadium-nitrogen alloy product.But nitriding is completely identical conventional solid-state nitriding method still, and the V/N value of the ferrovanadium nitride generating is still undesirable.
The production method of all kinds of ferrovanadium nitrides of prior art, or production process complexity causes benefit not high, or production process is simple but product quality is not ideal enough, and result of use is desirable not enough.
Summary of the invention
For overcoming the deficiencies in the prior art, the invention provides that a kind of production process is simple, high efficiency, the more preferably ferrovanadium nitride preparation method of high-quality low-cost of product quality amount.
The present invention for the technical scheme that reaches above-mentioned technical purpose and adopt is: a kind of ferrovanadium nitride preparation method of high-quality low-cost, and production process comprises the following steps:
A, first sieve after adopting respectively ball mill to grind vanadium-containing compound, carbon compound, nitrogen pick-up compound, promotor, crossing grit number is 80-120 order; Obtain vanadium-containing compound powder, carbon compound powder, nitrogen pick-up compound powder, promotor powder;
B, be that the vanadium-containing compound powder of 50-65 part, the carbon compound powder that weight part is 15-25 part, the nitrogen pick-up compound powder that weight part is 5-10 part, the accelerant powder that weight part is 10-22 part, the binding agent that weight part is 0.1-5 part, the water mixing and stirring that weight part is 5-10 part obtain mixture by weight part;
C, the mixture that B step is obtained utilize ball press to carry out pressure ball molding, and obtaining diameter is the ball block mixture of 5cm size;
D, ball block mixture is sent into temperature is to carry out drying and dehydrating processing in the dry attached kiln of 100-150 DEG C; The piece material that the dry processed of attached drying kiln drying is crossed is sent in main kiln, and first through calcining zone heating and calcining, calcining zone temperature control is 500-650 DEG C; After calcining, send into nitrogenize district, the temperature control of nitrogenize district is 1000-1250 DEG C, and it is 99.999% high pure nitrogen that nitrogenize district is filled with concentration of volume percent; And then send into flat-temperature zone, flat-temperature zone temperature control is 1250-1400 DEG C; Finally send into cooling zone, cooling zone temperature control is lower than 120 DEG C; Ball block mixture piece material is controlled as 20-22 hour to the total time that goes out main kiln from entering main kiln, and the piece material after coming out of the stove obtains product through screening.
Described vanadium-containing compound is wherein any mixture that is no less than two kinds of any in five kinds of Vanadium Pentoxide in FLAKESs, vanadous oxide, vanadium tetraoxide, ammonium poly-vanadate, ammonium meta-vanadate or they.
Described promotor is the mixture of any in two kinds of ferric oxide, iron powder or two kinds.
Described nitrogen pick-up compound is the mixture of any in two kinds of silicoaluminates, ferrosilicon or two kinds.
Described carbon compound is wherein any mixture that is no less than two kinds of any in four kinds of crystalline graphite powders, carbon black powder, wood charcoal powder, Graphite Electrodes carbon dust or they.
Described binding agent is wherein any mixture that is no less than two kinds of any in three kinds, flour, polyvinyl alcohol, starch or they.
Described main kiln is pushed bat kiln.
The invention has the beneficial effects as follows: can generate ferrovanadium nitride by a step sintering because material is uniformly mixed into the reactor of putting under nitrogen protection atmosphere after type; simple for process, workable, energy-saving and cost-reducing; invest lessly, can significantly improve the throughput of ferrovanadium nitride product.Because mixture comprises nitrogen pick-up compound, nitriding process can carry out in the material ball piece of mixing moulding simultaneously, therefore not be used under condition of high voltage and just can complete well, because the parameter such as temperature, time to sintering process is further optimized setting, production process is simple, high efficiency, product quality amount are better, and result of use is better.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
The 1st kind of embodiment of the present invention, a kind of ferrovanadium nitride preparation method of high-quality low-cost, production process comprises the following steps:
A, first sieve after adopting respectively ball mill to grind vanadium-containing compound, carbon compound, nitrogen pick-up compound, promotor, crossing grit number is 80 orders; Obtain vanadium-containing compound powder, carbon compound powder, nitrogen pick-up compound powder, promotor powder;
B, be that the vanadium-containing compound powder of 50 parts, the carbon compound powder that weight part is 15 parts, the nitrogen pick-up compound powder that weight part is 5 parts, the accelerant powder that weight part is 10 parts, the binding agent that weight part is 0.1 part, the water mixing and stirring that weight part is 5 parts obtain mixture by weight part;
C, the mixture that B step is obtained utilize ball press to carry out pressure ball molding, and obtaining diameter is the ball block mixture of 5cm size;
D, ball block mixture is sent into temperature is to carry out drying and dehydrating processing in the dry attached kiln of 100-150 DEG C; The piece material that the dry processed of attached drying kiln drying is crossed is sent in main kiln, and first through calcining zone heating and calcining, calcining zone temperature control is 500-650 DEG C; After calcining, send into nitrogenize district, the temperature control of nitrogenize district is 1000-1250 DEG C, and it is 99.999% high pure nitrogen that nitrogenize district is filled with concentration of volume percent; And then send into flat-temperature zone, flat-temperature zone temperature control is 1250-1400 DEG C; Finally send into cooling zone, cooling zone temperature control is lower than 120 DEG C; Ball block mixture piece material is controlled as 20-22 hour to the total time that goes out main kiln from entering main kiln, and the piece material after coming out of the stove obtains product through screening.
Described vanadium-containing compound is wherein any mixture that is no less than two kinds of any in five kinds of Vanadium Pentoxide in FLAKESs, vanadous oxide, vanadium tetraoxide, ammonium poly-vanadate, ammonium meta-vanadate or they.
Described promotor is the mixture of any in two kinds of ferric oxide, iron powder or two kinds.
Described nitrogen pick-up compound is the mixture of any in two kinds of silicoaluminates, ferrosilicon or two kinds.
Described carbon compound is wherein any mixture that is no less than two kinds of any in four kinds of crystalline graphite powders, carbon black powder, wood charcoal powder, Graphite Electrodes carbon dust or they.
Described binding agent is wherein any mixture that is no less than two kinds of any in three kinds, flour, polyvinyl alcohol, starch or they.
Described main kiln is pushed bat kiln.
The 2nd kind of embodiment of the present invention, a kind of ferrovanadium nitride preparation method of high-quality low-cost, production process comprises the following steps:
A, first sieve after adopting respectively ball mill to grind vanadium-containing compound, carbon compound, nitrogen pick-up compound, promotor, crossing grit number is 120 orders; Obtain vanadium-containing compound powder, carbon compound powder, nitrogen pick-up compound powder, promotor powder;
B, be that the vanadium-containing compound powder of 65 parts, the carbon compound powder that weight part is 25 parts, the nitrogen pick-up compound powder that weight part is 10 parts, the accelerant powder that weight part is 22 parts, the binding agent that weight part is 5 parts, the water mixing and stirring that weight part is 10 parts obtain mixture by weight part;
C, the mixture that B step is obtained utilize ball press to carry out pressure ball molding, and obtaining diameter is the ball block mixture of 5cm size;
D, ball block mixture is sent into temperature is to carry out drying and dehydrating processing in the dry attached kiln of 100-150 DEG C; The piece material that the dry processed of attached drying kiln drying is crossed is sent in main kiln, and first through calcining zone heating and calcining, calcining zone temperature control is 500-650 DEG C; After calcining, send into nitrogenize district, the temperature control of nitrogenize district is 1000-1250 DEG C, and it is 99.999% high pure nitrogen that nitrogenize district is filled with concentration of volume percent; And then send into flat-temperature zone, flat-temperature zone temperature control is 1250-1400 DEG C; Finally send into cooling zone, cooling zone temperature control is lower than 120 DEG C; Ball block mixture piece material is controlled as 20-22 hour to the total time that goes out main kiln from entering main kiln, and the piece material after coming out of the stove obtains product through screening.
Described vanadium-containing compound is wherein any mixture that is no less than two kinds of any in five kinds of Vanadium Pentoxide in FLAKESs, vanadous oxide, vanadium tetraoxide, ammonium poly-vanadate, ammonium meta-vanadate or they.
Described promotor is the mixture of any in two kinds of ferric oxide, iron powder or two kinds.
Described nitrogen pick-up compound is the mixture of any in two kinds of silicoaluminates, ferrosilicon or two kinds.
Described carbon compound is wherein any mixture that is no less than two kinds of any in four kinds of crystalline graphite powders, carbon black powder, wood charcoal powder, Graphite Electrodes carbon dust or they.
Described binding agent is wherein any mixture that is no less than two kinds of any in three kinds, flour, polyvinyl alcohol, starch or they.
Described main kiln is pushed bat kiln.
The 3rd kind of embodiment of the present invention.A ferrovanadium nitride preparation method for high-quality low-cost, production process comprises the following steps:
A, first sieve after adopting respectively ball mill to grind vanadium-containing compound, carbon compound, nitrogen pick-up compound, promotor, crossing grit number is 100 orders; Obtain vanadium-containing compound powder, carbon compound powder, nitrogen pick-up compound powder, promotor powder;
B, be that the vanadium-containing compound powder of 57 parts, the carbon compound powder that weight part is 20 parts, the nitrogen pick-up compound powder that weight part is 8 parts, the accelerant powder that weight part is 16 parts, the binding agent that weight part is 3 parts, the water mixing and stirring that weight part is 8 parts obtain mixture by weight part;
C, the mixture that B step is obtained utilize ball press to carry out pressure ball molding, and obtaining diameter is the ball block mixture of 5cm size;
D, ball block mixture is sent into temperature is to carry out drying and dehydrating processing in the dry attached kiln of 100-150 DEG C; The piece material that the dry processed of attached drying kiln drying is crossed is sent in main kiln, and first through calcining zone heating and calcining, calcining zone temperature control is 500-650 DEG C; After calcining, send into nitrogenize district, the temperature control of nitrogenize district is 1000-1250 DEG C, and it is 99.999% high pure nitrogen that nitrogenize district is filled with concentration of volume percent; And then send into flat-temperature zone, flat-temperature zone temperature control is 1250-1400 DEG C; Finally send into cooling zone, cooling zone temperature control is lower than 120 DEG C; Ball block mixture piece material is controlled as 20-22 hour to the total time that goes out main kiln from entering main kiln, and the piece material after coming out of the stove obtains product through screening.
Described vanadium-containing compound is wherein any mixture that is no less than two kinds of any in five kinds of Vanadium Pentoxide in FLAKESs, vanadous oxide, vanadium tetraoxide, ammonium poly-vanadate, ammonium meta-vanadate or they.
Described promotor is the mixture of any in two kinds of ferric oxide, iron powder or two kinds.
Described nitrogen pick-up compound is the mixture of any in two kinds of silicoaluminates, ferrosilicon or two kinds.
Described carbon compound is wherein any mixture that is no less than two kinds of any in four kinds of crystalline graphite powders, carbon black powder, wood charcoal powder, Graphite Electrodes carbon dust or they.
Described binding agent is wherein any mixture that is no less than two kinds of any in three kinds, flour, polyvinyl alcohol, starch or they.
Described main kiln is pushed bat kiln.
The product that the present invention finally obtains reaches following index after testing:
V：45％-55％；
N：12％-16％；
C：≤3％；
The V/N value of ferrovanadium nitride is about 3.7;
Product proportion is greater than 5g/cm
3.
Product main performance index can meet related request completely.
Claims (7)
1. a ferrovanadium nitride preparation method for high-quality low-cost, is characterized in that: production process comprises the following steps:
A, first sieve after adopting respectively ball mill to grind vanadium-containing compound, carbon compound, nitrogen pick-up compound, promotor, crossing grit number is 80-120 order; Obtain vanadium-containing compound powder, carbon compound powder, nitrogen pick-up compound powder, promotor powder;
B, be that the vanadium-containing compound powder of 50-65 part, the carbon compound powder that weight part is 15-25 part, the nitrogen pick-up compound powder that weight part is 5-10 part, the accelerant powder that weight part is 10-22 part, the binding agent that weight part is 0.1-5 part, the water mixing and stirring that weight part is 5-10 part obtain mixture by weight part;
C, the mixture that B step is obtained utilize ball press to carry out pressure ball molding, and obtaining diameter is the ball block mixture of 5cm size;
D, ball block mixture is sent into temperature is to carry out drying and dehydrating processing in the dry attached kiln of 100-150 DEG C; The piece material that the dry processed of attached drying kiln drying is crossed is sent in main kiln, and first through calcining zone heating and calcining, calcining zone temperature control is 500-650 DEG C; After calcining, send into nitrogenize district, the temperature control of nitrogenize district is 1000-1250 DEG C, and it is 99.999% high pure nitrogen that nitrogenize district is filled with concentration of volume percent; And then send into flat-temperature zone, flat-temperature zone temperature control is 1250-1400 DEG C; Finally send into cooling zone, cooling zone temperature control is lower than 120 DEG C; Ball block mixture piece material is controlled as 20-22 hour to the total time that goes out main kiln from entering main kiln, and the piece material after coming out of the stove obtains product through screening.
2. the ferrovanadium nitride preparation method of a kind of high-quality low-cost according to claim 1, is characterized in that: described vanadium-containing compound is wherein any mixture that is no less than two kinds of any in five kinds of Vanadium Pentoxide in FLAKESs, vanadous oxide, vanadium tetraoxide, ammonium poly-vanadate, ammonium meta-vanadate or they.
3. the ferrovanadium nitride preparation method of a kind of high-quality low-cost according to claim 1, is characterized in that: described promotor is the mixture of any in two kinds of ferric oxide, iron powder or two kinds.
4. the ferrovanadium nitride preparation method of a kind of high-quality low-cost according to claim 1, is characterized in that: described nitrogen pick-up compound is the mixture of any in two kinds of silicoaluminates, ferrosilicon or two kinds.
5. the ferrovanadium nitride preparation method of a kind of high-quality low-cost according to claim 1, is characterized in that: described carbon compound is wherein any mixture that is no less than two kinds of any in four kinds of crystalline graphite powders, carbon black powder, wood charcoal powder, Graphite Electrodes carbon dust or they.
6. the ferrovanadium nitride preparation method of a kind of high-quality low-cost according to claim 1, is characterized in that: described binding agent is wherein any mixture that is no less than two kinds of any in three kinds, flour, polyvinyl alcohol, starch or they.
7. according to the ferrovanadium nitride preparation method of a kind of high-quality low-cost described in any one in claim 1 to 6, it is characterized in that: described main kiln is pushed bat kiln.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105986163A (en) * | 2015-01-30 | 2016-10-05 | 新疆众豪钒业科技有限公司 | Nitrided ferrovanadium production method and apparatus |
| CN107974608A (en) * | 2017-11-20 | 2018-05-01 | 西安建筑科技大学 | A kind of ferrovanadium nitride and preparation method thereof |
| CN109136612A (en) * | 2018-09-25 | 2019-01-04 | 山东济钢合金材料科技有限公司 | A kind of preparation method of VN alloy |
| CN111020106A (en) * | 2019-12-13 | 2020-04-17 | 湖南众鑫新材料科技股份有限公司 | Vanadium-nitrogen alloy additive and preparation method thereof |
| CN113652570A (en) * | 2021-08-20 | 2021-11-16 | 湖南众鑫新材料科技股份有限公司 | Process for increasing nitrogen content of vanadium nitride iron |
| CN113736987A (en) * | 2021-08-02 | 2021-12-03 | 河钢承德钒钛新材料有限公司 | Preparation method of nitrided ferrovanadium alloy |
| CN113930661A (en) * | 2021-08-10 | 2022-01-14 | 河钢承德钒钛新材料有限公司 | Preparation method of nitrided ferrovanadium alloy additive |
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| CN103572086A (en) * | 2013-11-18 | 2014-02-12 | 福建新航凯材料科技有限公司 | Production method of manganese-vanadium nitride multicomponent alloy |
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2014
- 2014-05-15 CN CN201410205236.9A patent/CN104018056A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103572086A (en) * | 2013-11-18 | 2014-02-12 | 福建新航凯材料科技有限公司 | Production method of manganese-vanadium nitride multicomponent alloy |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105986163A (en) * | 2015-01-30 | 2016-10-05 | 新疆众豪钒业科技有限公司 | Nitrided ferrovanadium production method and apparatus |
| CN107974608A (en) * | 2017-11-20 | 2018-05-01 | 西安建筑科技大学 | A kind of ferrovanadium nitride and preparation method thereof |
| CN109136612A (en) * | 2018-09-25 | 2019-01-04 | 山东济钢合金材料科技有限公司 | A kind of preparation method of VN alloy |
| CN111020106A (en) * | 2019-12-13 | 2020-04-17 | 湖南众鑫新材料科技股份有限公司 | Vanadium-nitrogen alloy additive and preparation method thereof |
| CN111020106B (en) * | 2019-12-13 | 2021-07-27 | 湖南众鑫新材料科技股份有限公司 | Vanadium-nitrogen alloy additive and preparation method thereof |
| CN113736987A (en) * | 2021-08-02 | 2021-12-03 | 河钢承德钒钛新材料有限公司 | Preparation method of nitrided ferrovanadium alloy |
| CN113736987B (en) * | 2021-08-02 | 2023-11-28 | 河钢承德钒钛新材料有限公司 | Preparation method of nitrided ferrovanadium alloy |
| CN113930661A (en) * | 2021-08-10 | 2022-01-14 | 河钢承德钒钛新材料有限公司 | Preparation method of nitrided ferrovanadium alloy additive |
| CN113652570A (en) * | 2021-08-20 | 2021-11-16 | 湖南众鑫新材料科技股份有限公司 | Process for increasing nitrogen content of vanadium nitride iron |
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Application publication date: 20140903 |