CN106315524A - Method for producing vanadium nitride through pushed slab kiln - Google Patents
Method for producing vanadium nitride through pushed slab kiln Download PDFInfo
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- CN106315524A CN106315524A CN201610603742.2A CN201610603742A CN106315524A CN 106315524 A CN106315524 A CN 106315524A CN 201610603742 A CN201610603742 A CN 201610603742A CN 106315524 A CN106315524 A CN 106315524A
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- SKKMWRVAJNPLFY-UHFFFAOYSA-N azanylidynevanadium Chemical compound [V]#N SKKMWRVAJNPLFY-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 238000004519 manufacturing process Methods 0.000 title abstract description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 188
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 93
- 238000000034 method Methods 0.000 claims abstract description 39
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 17
- 230000009467 reduction Effects 0.000 claims abstract description 13
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 claims description 14
- 230000004044 response Effects 0.000 claims description 12
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 3
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 2
- 238000007599 discharging Methods 0.000 abstract description 5
- 239000003054 catalyst Substances 0.000 abstract description 4
- 230000008878 coupling Effects 0.000 abstract description 4
- 238000010168 coupling process Methods 0.000 abstract description 4
- 238000005859 coupling reaction Methods 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 4
- 230000006872 improvement Effects 0.000 abstract description 2
- 230000009977 dual effect Effects 0.000 abstract 1
- 239000008188 pellet Substances 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 abstract 1
- 230000035484 reaction time Effects 0.000 abstract 1
- 230000001360 synchronised effect Effects 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 19
- 239000002932 luster Substances 0.000 description 18
- 238000005516 engineering process Methods 0.000 description 13
- 238000006722 reduction reaction Methods 0.000 description 12
- 230000008569 process Effects 0.000 description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 8
- 239000000654 additive Substances 0.000 description 7
- 230000000996 additive effect Effects 0.000 description 7
- 238000012545 processing Methods 0.000 description 6
- GNTDGMZSJNCJKK-UHFFFAOYSA-N Vanadium(V) oxide Inorganic materials O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 229910021541 Vanadium(III) oxide Inorganic materials 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 4
- 229910052720 vanadium Inorganic materials 0.000 description 4
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 4
- 208000037656 Respiratory Sounds Diseases 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000002912 waste gas Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- YIWGJFPJRAEKMK-UHFFFAOYSA-N 1-(2H-benzotriazol-5-yl)-3-methyl-8-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carbonyl]-1,3,8-triazaspiro[4.5]decane-2,4-dione Chemical compound CN1C(=O)N(c2ccc3n[nH]nc3c2)C2(CCN(CC2)C(=O)c2cnc(NCc3cccc(OC(F)(F)F)c3)nc2)C1=O YIWGJFPJRAEKMK-UHFFFAOYSA-N 0.000 description 1
- 208000036626 Mental retardation Diseases 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000005121 nitriding Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0615—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium
- C01B21/0617—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium with vanadium, niobium or tantalum
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/10—Solid density
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a method for producing vanadium nitride through a pushed slab kiln. The method includes the following steps that 1, excessive iron powder is added in the material preparation process; 2, charging is carried out, wherein green pellets are charged into square charging buckets and round charging buckets put on a production line in a proportionally-mixed mode; 3, reduction nitridation is carried out, wherein the charging buckets pass through various temperature zones in the kiln after entering the kiln, the temperatures of the temperature zones and the flow of introduced nitrogen are controlled, the kiln cavity pressures at the kiln head, the kiln middle and the kiln tail are controlled, and a vanadium nitride product is obtained. According to the method, by increasing the catalyst proportion, changing the charging mode and adopting kiln temperature, nitrogen flow and kiln pressure synchronous coupling control, the quality and yield of vanadium nitride are effectively improved, the discharging speed is increased, the reaction time is shortened, and dual improvement of the yield of vanadium nitride produced through the pushed slab kiln and the product quality is achieved.
Description
Technical field
The present invention relates to a kind of method that pushed bat kiln produces vanadium nitride, belong to VN alloy production technical field.
Background technology
Pushed bat kiln is a kind of mature equipment producing vanadium nitride, is the capital equipment of current vanadium nitride production, domestic nitridation
Vanadium manufacturing enterprise the most all uses this equipment.During pushed bat kiln produces vanadium nitride, first by raw and auxiliary material by certain ratio
Pressure ball after example mixing, puts into graphite batch can by the green-ball obtained, under uniform temperature and condition of nitrogen gas, through certain time,
Make batch can feed from kiln hood, after kiln tail discharging, obtain vanadium nitride product.
At present, due to vanadium nitride Market competition, product price is on the low side, and therefore product cost and product quality just become
The most important condition of existence in the market competition, the main method reducing cost seeks to improve single kiln yield, improves product quality
Mainly improve product appearance and VN16 ratio.And single kiln yields poorly, product appearance is poor, the low the most current nitrogen of VN16 ratio
Change vanadium and produce the subject matter faced, how to solve these difficult problems and just seem very urgent, pushed bat kiln is produced vanadium nitride and also has
Significant.
The patent disclosure of Application No. 01139886.8 production method of a kind of vanadium nitride, the method is to be aoxidized by vanadium
After thing, graphite, the 2% uniform pressure ball of polyvinyl alcohol, join and be connected with protection and reacting gas nitrogen and/or the push pedal of ammonia
In kiln or tunnel cave, at a temperature of 1000-1800 DEG C, react 2-6h, discharging after being cooled to 100-250 DEG C.The method only discloses
The raw material composition of vanadium nitride and broad reaction temperature and response time, but not to the interpolation increased in throughput method, raw material
The kind of agent and consumption, nitrogen flow and high-temperature region temperature illustrate.
A kind of easy vanadium nitride production method of the patent disclosure of Application No. 201110000961.9, the method will
V2O5Powder and graphite powder add content by the weight ratio of 100: 15 after being sufficiently mixed on dry-mixed machine by the weight ratio of 4:1
The polyvinyl alcohol water solution of 4%, mixing, pressure ball, is dried, will be dried, by mixing sphere of powder layering loading truck, enter stove, Sealing furnace
Door, after being passed through nitrogen, after keeping 5h, 6h, 6-10h 20h altogether respectively at 800 DEG C, 1350 DEG C, 1600 DEG C, has a power failure under vacuum condition
It is cooled to 150 DEG C come out of the stove.This technology discloses accurate proportioning raw materials and response time, reaction temperature, but it uses very
Empty reaction, device therefor is not pushed bat kiln, and the most kind and consumption, nitrogen flow etc. to the additive in raw material are not said
Bright.
Although vanadium nitride production method and means are more at present, but use the vanadium nitride often surface matter of conventional method production
It is poor to measure, and nitrogen content is low, and the response time is long, yields poorly, and causes the cost of vanadium nitride product to remain high.
Summary of the invention
The present invention provides a kind of method that pushed bat kiln produces vanadium nitride, by improving catalyst ratio, changing charging method,
And use kiln temperature, nitrogen flow and furnace pressure to synchronize coupling control, it is effectively increased quality and the yield of vanadium nitride, increases discharging speed
Degree, shortens the response time, it is achieved that pushed bat kiln produces vanadium nitride yield and the double lifting of product quality.
The technical solution used in the present invention is:
A kind of pushed bat kiln produces the method for vanadium nitride, comprises the steps:
(1) excess iron powder is added during dispensing；
(2) charging: load green-ball to be mixed in proportion and throw in the square stock tank produced on line and circle batch can；
(3) reduction nitridation: after batch can enters kiln, each warm area in sequentially passing through kiln, control each warm area temperature respectively and be passed through nitrogen
Flow, and the kiln cavity pressure in kiln hood, kiln and at kiln tail is controlled, react under a nitrogen atmosphere, obtain vanadium nitride
Product.
The iron powder amount added in step (1) is 6-12kg/ ton barium oxide, preferably 8-10kg/ ton barium oxide.Conventional
In process of producing vanadium nitride, barium oxide per ton allocates 1-2Kg iron powder into as catalyst, promotes that synthetic reaction, the present invention exist
After research vanadium nitride course of reaction and product composition, iron powder addition is brought up to 6-12Kg/ ton barium oxide, significantly improves
During originally vanadium nitride produces, product density is low, and there is the problem of the apparent mass differences such as crackle on surface, and the product appearance of the present invention is bright and clean
Flawless, presents metallic luster, and apparent density arrives 3.5g/cm3Above, significantly improve it and make steel medium application effect.
In step (2), square stock tank mix, with circle batch can, the ratio thrown in producing on line is 1:1-4:1, preferably square stock tank and
It is 2:1 or 3:1 that circle batch can throws in ratio.The present invention side of employing, the circle mode of production that is used in mixed way of batch can, will enter kiln square stock tank and
Circle batch can is thrown in proportion, has both increased yield, has increased again product nitrogen content.After using circumference batch can mixed, due to square stock tank
Volume is more than circle batch can, it is possible to be effectively increased yield more than 25%；And after adding square stock tank, in making kiln, nitrogen circulation is become by advection
For turbulent flow, thus nitrogen distribution situation in improving kiln, beneficially product nitridation, make product nitrogen content improve more than 0.3%.
In step (3), temperature controls is 6 warm area 1000 DEG C-1100 DEG C；7-8 warm area 1100 DEG C-1350 DEG C；9 warm areas 1400
℃-1500℃；10-17 warm area 1510 DEG C-1540 DEG C.The present invention changes tradition kiln temperature distribution situation, before middle high-temperature region
Move, make 6 warm areas reach more than 1000 DEG C, reach more than 1300 DEG C to 8 warm areas, the most also Accelerating reduction course of reaction；Through 9 warm areas
After high temperature transition, high temperature warm area is advanced to 10th district, controls 10-17 warm area temperature more than 1510 DEG C, enhanced products nitrogenizing effect,
Extend the response time, be effectively improved yield.
The nitrogen flow that in step (3), each warm area is passed through controls: 1-5 warm area 3500-4000 L/min；6-8 warm area
5000-5800L/min；9 warm area 6000-6500L/min, 10 warm areas and later 6500-8000 L/min；It is preferably each warm area to lead to
The nitrogen flow entered controls: 1-5 warm area 3600 L/min-3800 L/min；6-8 warm area 5300-5500 L/min；9 temperature
District 6300L/min, 10 warm areas and later 7000-7500 L/min.Adjusting nitrogen amount according to each section of reaction requirement, 1-5 warm area is low
Nitrogen flow, is only sufficient to ensure nitrogen atmosphere in kiln, it is easy to moisture evaporation and waste gas discharge, in 6-9 warm area reduction process, along with kiln
Temperature rise, incrementally increases nitrogen flow, it is ensured that reduction effect, and main generation vanadium nitride reaction after 10 warm areas, by nitrogen flow
All open to 7000 more than L/min, increase this section nitrogen partial pressure, accelerate response speed, shorten the response time, improve yield.
In step (3), pressure control is: kiln hood pressure 1-10Pa, pressure 5-20Pa in kiln, kiln tail pressure 8-20Pa, nitrogen
Under the conditions of the response time be 13-15h.It is preferably, kiln hood pressure 4-6Pa, pressure 10-15Pa in kiln, kiln tail pressure 14-16Pa.
The present invention creates pressure control technology, by reacting in monitoring pressure control kiln.In the low furnace pressure of kiln hood, beneficially useless gas and water in kiln
Vapour circulates to kiln hood, it is simple to discharged by chimney in time；The large quantity of exhaust gas that in kiln, reduction reaction is released is unfavorable for that reduction and nitriding are anti-
Should carry out, how many by exhausted air quantity in furnace pressure checking kiln, ensure that waste gas is the most normally discharged by controlling furnace pressure, promote reduction and ooze
Nitrogen response speed, it is ensured that carry product；Kiln tail furnace pressure can regard nitrogen pressure as, controls kiln tail furnace pressure and ensures nitrogen partial pressure in stove, increases
Product is nitrogenous, improves product quality.
Use and have the beneficial effects that produced by technique scheme:
By improving catalyst ratio, changing charging method, and use kiln temperature, nitrogen flow and furnace pressure to synchronize coupling control, have
Effect improves quality and the yield of vanadium nitride, increases discharging speed, shortens the response time, it is achieved that pushed bat kiln produces vanadium nitride and produces
Amount and the double lifting of product quality.
The present invention synchronizes coupling by kiln temperature, nitrogen flow and furnace pressure and controls, and shortens the response time to greatest extent, increases and
Material speed, is effectively increased pushed bat kiln yield, and achieves pushed bat kiln production vanadium nitride yield and the double lifting of product quality.
The apparent flawless of vanadium nitride product that this method produces, metal luster, apparent density arrives 3.5g/cm3Above,
Product entirely reaches VN16 standard, single pushed bat kiln list kiln daily output up to more than 1.5 tons, the dou-ble-pusher kiln list kiln daily output up to
More than 3.0 tons, substantially increase yield.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described further；
Embodiment 1:
Following processing step is used to improve vanadium nitride yield and product quality:
(1) dispensing: 1 ton of Vanadium sesquioxide and 280Kg graphite powder are mixed and allocate into iron powder 8kg and makees additive；
(2) feed: green-ball is loaded and throws in the square stock tank produced on line and circle batch can in the mixing of 2:1 ratio；
(3) reduction nitridation: after batch can enters kiln, each warm area in sequentially passing through kiln, control each warm area temperature respectively, 6 warm areas 1000 DEG C,
7 warm areas 1100 DEG C, 8 warm area 1300 DEG C, 9 warm area 1450 DEG C, 10-17 warm area 1520 DEG C；The flow controlling to be passed through nitrogen is 1-5 temperature
District 3600L/min, 6-8 warm area 5300L/min, 9 warm area nitrogen flows are 6300L/min, and 10 warm areas and later nitrogen flow are
7000 L/min；Control kiln hood pressure 4Pa, pressure 10Pa in kiln, kiln tail pressure 14Pa；14h is reacted under the conditions of high temperature nitrogen,
To high yield, high-quality vanadium nitride.Product is apparent metallic luster and flawless, apparent density 3.53g/cm3, single kiln daily output
1.58 tons, product nitrogen content 15.63%, entirely reach VN16 standard.
Embodiment 2:
Following processing step is used to improve vanadium nitride yield and product quality:
(1) dispensing: 1 ton of Vanadium sesquioxide and 275Kg graphite powder are mixed and allocate into iron powder 10kg and makees additive；
(2) feed: green-ball is loaded and throws in the square stock tank produced on line and circle batch can in the mixing of 3:1 ratio；
(3) reduction nitridation: after batch can enters kiln, each warm area in sequentially passing through kiln, control each warm area temperature respectively, 6 warm areas 1100 DEG C,
7 warm areas 1200 DEG C, 8 warm area 1350 DEG C, 9 warm area 1450 DEG C, 10-17 warm area 1530 DEG C；The flow controlling to be passed through nitrogen is 1-5 temperature
District 3800L/min, 6-8 warm area 5500L/min, 9 warm area nitrogen flows are 6300L/min, and 10 warm areas and later nitrogen flow are
7500 L/min；Control kiln hood pressure 6Pa, pressure 15Pa in kiln, kiln tail pressure 16Pa；15h is reacted under the conditions of high temperature nitrogen,
To high yield, high-quality vanadium nitride.Product is apparent metallic luster and flawless, apparent density 3.58g/cm3, single kiln daily output
1.63 tons, product nitrogen content 15.42%, entirely reach VN16 standard.
Embodiment 3:
Following processing step is used to improve vanadium nitride yield and product quality:
(1) dispensing: 1 ton of vanadic anhydride and 350Kg graphite powder are mixed and allocate into iron powder 6kg and makees additive；
(2) feed: green-ball is loaded and throws in the square stock tank produced on line and circle batch can in the mixing of 1:1 ratio；
(3) reduction nitridation: after batch can enters kiln, each warm area in sequentially passing through kiln, control each warm area temperature respectively, 6 warm areas 1000 DEG C,
7 warm areas 1100 DEG C, 8 warm area 1200 DEG C, 9 warm area 1400 DEG C, 10-17 warm area 1510 DEG C；The flow controlling to be passed through nitrogen is 1-5 temperature
District 3500L/min, 6-8 warm area 5000L/min, 9 warm area nitrogen flows are 6000L/min, and 10 warm areas and later nitrogen flow are
6500 L/min；Control kiln hood pressure 10Pa, pressure 20Pa in kiln, kiln tail pressure 8Pa；13h is reacted under the conditions of high temperature nitrogen,
To high yield, high-quality vanadium nitride.Product is apparent metallic luster and flawless, apparent density 3.5g/cm3, single kiln daily output 1.5
Ton, product nitrogen content 14.45%, entirely reach VN16 standard.
Embodiment 4:
Following processing step is used to improve vanadium nitride yield and product quality:
(1) dispensing: 1 ton of vanadic anhydride and 355Kg graphite powder are mixed and allocate into iron powder 12kg and makees additive；
(2) feed: green-ball is loaded and throws in the square stock tank produced on line and circle batch can in the mixing of 4:1 ratio；
(3) reduction nitridation: after batch can enters kiln, each warm area in sequentially passing through kiln, control each warm area temperature respectively, 6 warm areas 1100 DEG C,
7 warm areas 1200 DEG C, 8 warm area 1350 DEG C, 9 warm area 1500 DEG C, 10-17 warm area 1540 DEG C；The flow controlling to be passed through nitrogen is 1-5 temperature
District 4000L/min, 6-8 warm area 5800L/min, 9 warm area nitrogen flows are 6500L/min, and 10 warm areas and later nitrogen flow are
8000 L/min；Control kiln hood pressure 1Pa, pressure 5Pa in kiln, kiln tail pressure 20Pa；Obtain high yield, high-quality vanadium nitride.
Product is apparent metallic luster and flawless, apparent density 3.62g/cm3, single kiln daily output 1.72 tons, product nitrogen content 14.12%,
Entirely reach VN16 standard.
Embodiment 5
Following processing step is used to improve vanadium nitride yield and product quality:
(1) dispensing: 1 ton of Vanadium sesquioxide and 280Kg graphite powder are mixed and allocate into iron powder 7kg and makees additive；
(2) feed: green-ball is loaded and throws in the square stock tank produced on line and circle batch can in the mixing of 2:1 ratio；
(3) reduction nitridation: after batch can enters kiln, each warm area in sequentially passing through kiln, control each warm area temperature respectively, 6 warm areas 1050 DEG C,
7 warm areas 1300 DEG C, 8 warm area 1350 DEG C, 9 warm area 1500 DEG C, 10-17 warm area 1520 DEG C；The flow controlling to be passed through nitrogen is 1-5 temperature
District 3800L/min, 6-8 warm area 5400L/min, 9 warm area nitrogen flows are 6500L/min, and 10 warm areas and later nitrogen flow are
6500 L/min；Control kiln hood pressure 5Pa, pressure 18Pa in kiln, kiln tail pressure 10Pa；15h is reacted under the conditions of high temperature nitrogen,
To high yield, high-quality vanadium nitride.Product is apparent metallic luster and flawless, apparent density 3.58g/cm3, single kiln daily output
1.70 tons, product nitrogen content 14.15%, entirely reach VN16 standard.
Embodiment 6
Following processing step is used to improve vanadium nitride yield and product quality:
(1) dispensing: 1 ton of Vanadium sesquioxide and 275Kg graphite powder are mixed and allocate into iron powder 11kg and makees additive；
(2) feed: green-ball is loaded and throws in the square stock tank produced on line and circle batch can in the mixing of 3:1 ratio；
(3) reduction nitridation: after batch can enters kiln, each warm area in sequentially passing through kiln, control each warm area temperature respectively, 6 warm areas 1080 DEG C,
7 warm areas 1250 DEG C, 8 warm area 1300 DEG C, 9 warm area 1450 DEG C, 10-17 warm area 1540 DEG C；The flow controlling to be passed through nitrogen is 1-5 temperature
District 4000L/min, 6-8 warm area 5600L/min, 9 warm area nitrogen flows are 6400L/min, and 10 warm areas and later nitrogen flow are
7800 L/min；Control kiln hood pressure 8Pa, pressure 8Pa in kiln, kiln tail pressure 18Pa；13h is reacted under the conditions of high temperature nitrogen,
To high yield, high-quality vanadium nitride.Product is apparent metallic luster and flawless, apparent density 3.61g/cm3, single kiln daily output
1.73 tons, product nitrogen content 14.13%, entirely reach VN16 standard.
Comparative example 1:
This comparative example is in addition to 1kg except dispensing adds iron powder amount, other batch cans throw in ratio and technology controlling and process all with embodiment 1 phase
Apparent without metallic luster and there is crackle with, product, apparent density 3.42g/cm3, single kiln daily output 1.51 tons, product nitrogen content
15.42%, entirely reach VN16 standard.
Comparative example 2:
This comparative example is in addition to 15kg except dispensing adds iron powder amount, other batch cans throw in ratio and technology controlling and process all with embodiment 1
Identical, product is apparent metallic luster and flawless, apparent density 3.7g/cm3, single kiln is produced daily up to 1.61 tons, but product contains
Vanadium 76.87, less than Standard, product is defective.
Comparative example 3:
This comparative example is thrown in addition to ratio be only to throw in round batch can except square stock tank and circle batch can, dispensing and other technology controlling and process all with
Embodiment 1 is identical, and product is apparent metallic luster and flawless, apparent density 3.51g/cm3, single kiln daily output 1.43 tons, product
Nitrogen content 14.77%, entirely reaches VN16 standard, yield and nitrogen content and decreases.
Comparative example 4:
Throwing in ratio except square stock tank and circle batch can in this comparative example be only in addition to input square stock tank, dispensing and other technology controlling and process all with
Embodiment 1 is identical, and product is apparent metallic luster and flawless, apparent density 3.51g/cm3, single kiln daily output 1.69 tons, product
Nitrogen content 14.06%, entirely reaches VN16 standard, and yield is greatly improved but product nitrogen content is greatly reduced, and product quality reduces relatively
Greatly.
Comparative example 5:
In this comparative example except 6 warm area 750 DEG C, 7 warm area 950 DEG C, 8 warm area 1100 DEG C, 9 warm area 1200 DEG C, 10 warm area 1350 DEG C, 11
Warm area 1450 DEG C (i.e. high-temperature region is from the beginning of 12 warm areas) outward, dispensing, batch can throw in ratio and other technology controlling and process all with embodiment 1
Identical, product is apparent metallic luster and flawless, apparent density 3.22g/cm3, single kiln daily output 1.51 tons, product nitrogen content
13.2%, for VN12, product nitrogen content and apparent density decline to a great extent.
Comparative example 6:
This comparative example i.e. increases low-temperature space nitrogen flow except 1-5 warm area nitrogen flow becomes 5500L/min() in addition to, dispensing, material
Ratio thrown in by tank and other technology controlling and process is the most same as in Example 1, and product is apparent metallic luster and flawless, apparent density
3.52g/cm3, single kiln daily output 1.51 tons, product nitrogen content 15.01%, entirely reach VN16 standard, but owing to waste gas is discharged too late
Time impact nitridation, product nitrogen content is declined slightly.
Comparative example 7:
This comparative example i.e. reduces high temperature and later warm area nitrogen flow except 10 warm areas nitrogen flow later becomes 5500L/min()
Outward, dispensing, batch can throw in ratio and other technology controlling and process is the most same as in Example 1, and product is apparent metallic luster and flawless,
Apparent density 3.52g/cm3, single kiln daily output 1.51 tons, product nitrogen content 14.23%, entirely reach VN16 standard, but product is nitrogenous
Amount declines to a great extent.
Comparative example 8:
Except controlling kiln hood pressure 14Pa, pressure 40Pa in kiln, kiln tail pressure 34Pa in this comparative example, remaining dispensing, batch can are thrown in
Ratio and other technology controlling and process are the most same as in Example 1, and product is apparent metallic luster and flawless, apparent density 3.52g/
cm3, single kiln daily output 1.51 tons, product nitrogen content 12.53%, product is VN12, and product nitrogen content declines to a great extent, and has a strong impact on product
Quality.
Comparative example 9:
Except controlling kiln hood pressure 1Pa, pressure 1Pa in kiln, kiln tail pressure 1Pa in this comparative example, remaining dispensing, batch can throw in ratio
And other technology controlling and process is the most same as in Example 1, product is apparent metallic luster and flawless, but has oxidative phenomena, apparent close
Degree 3.52g/cm3, single kiln daily output 1.51 tons, product nitrogen content 12.75%, product is VN12, and product nitrogen content declines to a great extent, sternly
Ghost image rings product quality.
Integrated embodiment 1-6 and comparative example 1-9 result are it can be seen that the present invention substantially increases pushed bat kiln yield, and energy
Enough improve nitrogen content and the apparent density of vanadium nitride, reduce product crackle and make product show metallic luster, thus improve
The quality of vanadium nitride.
The present invention defining, addition iron powder amount, to 6-12kg/ ton barium oxide, is crossed mental retardation and produced qualified products but table
Appearance quality is poor, too high, easily causes product defective；The side of defining, the input ratio of circle batch can are 1:1 ~ 4:1, do not put square stock tank
Or square stock tank the most all can cause product nitrogen content to reduce because of nitrogen irrational distribution；And by middle high-temperature region in advance, control 6 warm areas
Temperature 1000 DEG C-1100 DEG C；7-8 warm area controls temperature at 1100 DEG C-1350 DEG C；9 warm areas control temperature at 1400 DEG C-1500
℃；10-17 warm area controls temperature can make in the case of load is constant at 1510 DEG C-1540 DEG C that product is nitrogenous to be promoted by VN12
To VN16 standard；And nitrogen flow is set as that 1-5 warm area nitrogen flow is 3500-4000 L/min；6-8 warm area nitrogen flow is
5000-5800L/min；9 warm area nitrogen flows are 6000-6500L/min, and 10 warm areas and later nitrogen flow are 6500-8000
L/min, more preferably 1-5 warm area nitrogen flow is 3600 L/min-3800 L/min；6-8 warm area warm area nitrogen stream
Amount: 5300-5500 L/min；9 warm area nitrogen flows are 6300L/min, and 10 warm areas and later nitrogen flow are 7000-7500
During L/min, product nitrogen content is higher, increases or reduces nitrogen flow and product nitrogen content all can be caused to reduce；And pressure control kiln
Head pressure 1-10Pa, pressure 5-20Pa in kiln, kiln tail pressure 8-20Pa more preferably: kiln hood pressure 4-6Pa, pressure in kiln
10-15Pa, after kiln tail pressure 14-16Pa, the nitrogenous height of product, and increase or reduce furnace pressure, then product nitrogen content can be caused to decline
Until VN12 product occurs；
Therefore use this technology pushed bat kiln to produce vanadium nitride, pushed bat kiln yield, single pushed bat kiln list kiln daily output can be effectively increased
Up to more than 1.5 tons, the dou-ble-pusher kiln list kiln daily output is up to more than 3.0 tons；And the apparent flawless of product can be made, in metal light
Pool, apparent density arrives 3.5g/cm3Above, all VN16 of product.
The present invention illustrates the method detailed of the present invention by above-described embodiment, but the invention is not limited in above-mentioned in detail
Method, does not i.e. mean that the present invention has to rely on above-mentioned method detailed and could implement.Person of ordinary skill in the field should
Understanding, any improvement in the present invention, the equivalence of raw material each to product of the present invention is replaced and the interpolation of auxiliary element, concrete mode
Selection etc., all fall within protection scope of the present invention and open within the scope of.
Claims (10)
1. the method that a pushed bat kiln produces vanadium nitride, it is characterised in that: comprise the steps:
(1) excess iron powder is added during dispensing；
(2) charging: use square stock tank and circle batch can mixing charging method, green-ball is loaded and is mixed in proportion input on product line
In square stock tank and circle batch can；
(3) reduction nitridation: after batch can enters kiln, each warm area in sequentially passing through kiln, control each warm area temperature respectively and be passed through nitrogen
Flow, and the kiln cavity pressure in kiln hood, kiln and at kiln tail is controlled, react under a nitrogen atmosphere, obtain vanadium nitride
Product.
A kind of pushed bat kiln the most according to claim 1 produces the method for vanadium nitride, it is characterised in that described step adds in (1)
The iron powder amount entered is 6-12kg/ ton barium oxide.
A kind of pushed bat kiln the most according to claim 2 produces the method for vanadium nitride, it is characterised in that described step adds in (1)
The iron powder amount entered is 8-10kg/ ton barium oxide.
A kind of pushed bat kiln the most according to claim 1 produces the method for vanadium nitride, it is characterised in that side in described step (2)
It is 1:1-4:1 that batch can mixes, with circle batch can, the ratio thrown in producing on line.
A kind of pushed bat kiln the most according to claim 1 produces the method for vanadium nitride, it is characterised in that side in described step (2)
It is 2:1 or 3:1 that batch can throws in ratio with circle batch can.
A kind of pushed bat kiln the most according to claim 1 produces the method for vanadium nitride, it is characterised in that described step (3) middle temperature
Degree control is 6 warm area 1000 DEG C-1100 DEG C；7-8 warm area 1100 DEG C-1350 DEG C；9 warm areas 1400 DEG C-1500 DEG C；10-17 warm area
1510℃-1540℃。
A kind of pushed bat kiln the most according to claim 1 produces the method for vanadium nitride, it is characterised in that each in described step (3)
The nitrogen flow that warm area is passed through controls: 1-5 warm area 3500-4000 L/min；6-8 warm area 5000-5800L/min；9 warm areas
6000-6500L/min, 10 warm areas and later 6500-8000 L/min.
A kind of pushed bat kiln the most according to claim 7 produces the method for vanadium nitride, it is characterised in that each in described step (3)
The nitrogen flow that warm area is passed through controls: 1-5 warm area 3600 L/min-3800 L/min；6-8 warm area 5300-5500 L/
min；9 warm area 6300L/min, 10 warm areas and later 7000-7500 L/min.
A kind of pushed bat kiln the most according to claim 1 produces the method for vanadium nitride, it is characterised in that kiln in described step (3)
Voltage-controlled it is made as: kiln hood pressure 1-10Pa, pressure 5-20Pa in kiln, kiln tail pressure 8-20Pa, the condition of nitrogen gas lower response time is 13-
15h。
A kind of pushed bat kiln the most according to claim 9 produces the method for vanadium nitride, it is characterised in that in described step (3)
Pressure control is: kiln hood pressure 4-6Pa, pressure 10-15Pa in kiln, kiln tail pressure 14-16Pa.
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| 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 |
| CN108018474A (en) * | 2017-11-09 | 2018-05-11 | 中国电子科技集团公司第四十八研究所 | A kind of method that vanadium nitride is prepared with ammonium metavanadate serialization |
| CN108862215A (en) * | 2018-07-26 | 2018-11-23 | 河钢股份有限公司承德分公司 | A kind of production vanadium nitride binder and preparation method thereof |
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