CN106315524B - A kind of method of pushed bat kiln production vanadium nitride - Google Patents
A kind of method of pushed bat kiln production vanadium nitride Download PDFInfo
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- CN106315524B CN106315524B CN201610603742.2A CN201610603742A CN106315524B CN 106315524 B CN106315524 B CN 106315524B CN 201610603742 A CN201610603742 A CN 201610603742A CN 106315524 B CN106315524 B CN 106315524B
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- SKKMWRVAJNPLFY-UHFFFAOYSA-N azanylidynevanadium Chemical compound [V]#N SKKMWRVAJNPLFY-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 37
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 28
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 194
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 96
- 239000004615 ingredient Substances 0.000 claims abstract description 17
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 16
- 230000009467 reduction Effects 0.000 claims abstract description 14
- 230000035484 reaction time Effects 0.000 claims abstract description 11
- QUEDYRXQWSDKKG-UHFFFAOYSA-M [O-2].[O-2].[V+5].[OH-] Chemical compound [O-2].[O-2].[V+5].[OH-] QUEDYRXQWSDKKG-UHFFFAOYSA-M 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 3
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 2
- 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
- 238000007599 discharging Methods 0.000 abstract description 4
- 230000001360 synchronised effect Effects 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 19
- 239000002932 luster Substances 0.000 description 18
- 238000006722 reduction reaction Methods 0.000 description 14
- 238000005516 engineering process Methods 0.000 description 12
- 230000008569 process Effects 0.000 description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 9
- 239000000654 additive Substances 0.000 description 7
- 230000000996 additive effect Effects 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 7
- 229910052720 vanadium Inorganic materials 0.000 description 7
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 7
- 239000007789 gas Substances 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
- 208000037656 Respiratory Sounds Diseases 0.000 description 4
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 4
- CSSYLTMKCUORDA-UHFFFAOYSA-N barium(2+);oxygen(2-) Chemical class [O-2].[Ba+2] CSSYLTMKCUORDA-UHFFFAOYSA-N 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000203 mixture 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
- 230000007423 decrease Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000000463 material 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
- 230000036632 reaction speed Effects 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
- 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
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000006872 improvement Effects 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
- 239000012495 reaction gas Substances 0.000 description 1
- 238000011946 reduction process 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 kind of methods of pushed bat kiln production vanadium nitride, include the following steps: that excess iron powder is added when (1) ingredient；(2) it charges: green-ball being fitted into the square stock tank and circle batch can that mixing in proportion is launched in producing line；(3) reduction nitridation: after batch can enters kiln, successively by each warm area in kiln, each warm area temperature is controlled respectively and is passed through the flow of nitrogen, and the furnace chamber pressure in kiln hood, kiln and at kiln tail is controlled, obtains vanadium nitride product.The present invention is by improving catalyst ratio, changing charging method, and using the synchronous coupling control of kiln temperature, nitrogen flow and furnace pressure, the quality and yield of vanadium nitride are effectively increased, discharging speed is increased, shorten the reaction time, realizes pushed bat kiln production vanadium nitride yield and the double promotions of product quality.
Description
Technical field
The present invention relates to a kind of methods of pushed bat kiln production vanadium nitride, belong to VN alloy production technical field.
Background technique
Pushed bat kiln is a kind of mature equipment for producing vanadium nitride, is the capital equipment of current vanadium nitride production, country's nitridation
Vanadium manufacturing enterprise all uses this equipment substantially.During pushed bat kiln produces vanadium nitride, raw and auxiliary material is first pressed into certain ratio
Pressure ball after example mixes, obtained green-ball is put into graphite batch can, under certain temperature and condition of nitrogen gas, by certain time,
It feeds batch can from kiln hood, after kiln tail discharging, obtains vanadium nitride product.
Currently, product price is relatively low due to vanadium nitride Market competition, therefore product cost and product quality just become
The most important condition survived in market competition, the main method for reducing cost seek to improve single kiln yield, improve product quality
Mainly improve product appearance and VN16 ratio.And single kiln low output, product appearance are poor, the low also exactly current nitrogen of VN16 ratio
Change vanadium and produce the main problem faced, how to solve these problems just seems very urgent, also has to pushed bat kiln production vanadium nitride
It is significant.
Application No. is a kind of production methods of vanadium nitride of 01139886.8 patent disclosure, and this method is to aoxidize vanadium
After object, graphite, the uniform pressure ball of 2% polyvinyl alcohol, it is added to the push plate for being connected with protection and reaction gas nitrogen and/or ammonia
In kiln or tunnel oven, 2-6h is reacted at a temperature of 1000-1800 DEG C, is discharged after being cooled to 100-250 DEG C.This method only discloses
The raw material composition of vanadium nitride and broad reaction temperature and reaction time, but not to the addition in increase throughput method, raw material
The type and dosage of agent, nitrogen flow and high-temperature region temperature are illustrated.
Application No. is a kind of easy vanadium nitride production method of 201110000961.9 patent disclosure, this method will
V2O5Content is added by 100: 15 weight ratio after being sufficiently mixed on dry-mixed machine by the weight ratio of 4:1 in powder and graphite powder
Mixing sphere of powder layering is packed into truck, enters furnace, Sealing furnace by 4% polyvinyl alcohol water solution, mixing, pressure ball, drying after drying
, after being passed through nitrogen under vacuum condition, after 800 DEG C, 1350 DEG C, 1600 DEG C keep the total 20h of 5h, 6h, 6-10h respectively, have a power failure
150 DEG C are cooled to come out of the stove.The technology discloses accurate raw material proportioning and reaction time, reaction temperature, but it is used very
Sky reaction, device therefor is not pushed bat kiln, and also the type to the additive in raw material and dosage, nitrogen flow etc. are not said
It is bright.
Although vanadium nitride production method and means are more at present, using the vanadium nitride often surface matter of conventional method production
It is poor to measure, and nitrogen content is low, and the reaction time is long, low output, causes the cost of vanadium nitride product high.
Summary of the invention
The present invention provides a kind of method of pushed bat kiln production vanadium nitride, by improving catalyst ratio, changing charging method,
And using the synchronous coupling control of kiln temperature, nitrogen flow and furnace pressure, the quality and yield of vanadium nitride are effectively increased, discharging speed is increased
Degree shortens the reaction time, realizes pushed bat kiln production vanadium nitride yield and the double promotions of product quality.
The technical solution used in the present invention is:
A kind of method of pushed bat kiln production vanadium nitride, includes the following steps:
(1) excess iron powder is added when ingredient；
(2) it charges: green-ball being fitted into the square stock tank and circle batch can that mixing in proportion is launched in producing line；
(3) reduction nitridation: after batch can enters kiln, successively by each warm area in kiln, each warm area temperature is controlled respectively and is passed through nitrogen
The flow of gas, and the furnace chamber pressure in kiln hood, kiln and at kiln tail is controlled, it is reacted under a nitrogen atmosphere, obtains nitrogen
Change vanadium product.
The iron powder amount being added in step (1) is 6-12kg/ tons of barium oxides, preferably 8-10kg/ tons of barium oxide.It is conventional
In process of producing vanadium nitride, barium oxide supplying 1-2Kg iron powder per ton is as catalyst, and to promote synthetic reaction, the present invention exists
After studying vanadium nitride reaction process and product composition, iron powder additional amount is increased to 6-12Kg/ tons of barium oxides, is significantly improved
Originally product density is low in vanadium nitride production, and there is the problem of the apparent masses such as crackle difference on surface, and product appearance of the invention is bright and clean
Flawless, is presented metallic luster, and apparent density reaches 3.5g/cm3More than, it significantly improves it and is making steel medium application effect.
It is 1:1-4:1 that square stock tank, which mix the ratio in producing line of dispensing with circle batch can, in step (2), preferably square stock tank and
It is 2:1 or 3:1 that circle batch can, which launches ratio,.Present invention use side, the production method that is used in mixed way of circle batch can, will enter kiln square stock tank with
Circle batch can is launched in proportion, not only increases yield, but also increase product nitrogen content.After being used with using circumference batch can, due to square stock tank
Volume is greater than circle batch can, can effectively increase 25% or more yield；And after square stock tank is added, become nitrogen circulation in kiln by advection
It is conducive to product so as to improve nitrogen distribution situation in kiln for turbulent flow and nitrogenizes, product nitrogen content is made to improve 0.3% or more.
Temperature control is 1000 DEG C -1100 DEG C of 6 warm area in step (3)；1100 DEG C -1350 DEG C of 7-8 warm area；9 warm areas 1400
℃-1500℃；1510 DEG C -1540 DEG C of 10-17 warm area.The present invention changes traditional kiln temperature distribution situation, before high temperature area
It moves, 6 warm areas is made to reach 1000 DEG C or more, until 8 warm areas reach 1300 DEG C or more, ahead of time and Accelerating reduction reaction process；Through 9 warm areas
After high temperature transition, high temperature warm area is advanced to 10th area, 1510 DEG C of 10-17 warm area temperature of control or more, enhanced products nitrogenizing effect,
Extend the reaction time, effectively improves yield.
The nitrogen flow control that each warm area is passed through in step (3) are as follows: 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；Preferably each warm area is logical
The nitrogen flow control entered are as follows: 3600 L/min -3800 L/min of 1-5 warm area；6-8 warm area 5300-5500 L/min；9 temperature
Area 6300L/min, 10 warm areas and later 7000-7500 L/min.Nitrogen amount is adjusted according to each section of reaction requirement, 1-5 warm area is low
Nitrogen flow is only sufficient to guarantee nitrogen atmosphere in kiln, is easy to moisture evaporation and exhaust gas discharges, in 6-9 warm area reduction process, with kiln
Temperature increases, and incrementally increases nitrogen flow, guarantees reduction effect, later vanadium nitride reaction mainly occurs for 10 warm areas, by nitrogen flow
It all opens to 7000 L/min or more, increases this section nitrogen partial pressure, accelerate reaction speed, shorten the reaction time, improve yield.
Pressure control in step (3) are as follows: kiln hood pressure 1-10Pa, pressure 5-20Pa in kiln, kiln tail pressure 8-20Pa, nitrogen
Under the conditions of the reaction time be 13-15h.Preferably, kiln hood pressure 4-6Pa, pressure 10-15Pa, kiln tail pressure 14-16Pa in kiln.
The present invention creates pressure control technology, by reacting in monitoring pressure control kiln.In the low furnace pressure of kiln hood, it is conducive to gas and water of giving up in kiln
Vapour circulates to kiln hood, convenient for being discharged in time by chimney；The large quantity of exhaust gas that reduction reaction is released in kiln is unfavorable for reduction and nitriding is anti-
Should carry out, by furnace pressure verify kiln in exhausted air quantity how much, by control furnace pressure guarantee exhaust gas be normally discharged, promote reduction and seep
Nitrogen reaction speed, it is ensured that propose production；Kiln tail furnace pressure can regard nitrogen pressure as, and control kiln tail furnace pressure guarantees nitrogen partial pressure in furnace, increases
Product is nitrogenous, improves product quality.
The beneficial effects of adopting the technical scheme are that
By improving catalyst ratio, changing charging method, and using the synchronous coupling control of kiln temperature, nitrogen flow and furnace pressure
System effectively increases the quality and yield of vanadium nitride, increases discharging speed, shortens the reaction time, realizes pushed bat kiln production nitrogen
Change vanadium yield and the double promotions of product quality.
The present invention is shortened the reaction time to greatest extent, is increased out by the synchronous coupling control of kiln temperature, nitrogen flow and furnace pressure
Expect speed, effectively increase pushed bat kiln yield, and realizes pushed bat kiln production vanadium nitride yield and the double promotions of product quality.
The apparent flawless of vanadium nitride product of this method production, metal luster, apparent density reach 3.5g/cm3More than,
Product entirely reaches VN16 standard, and for single pushed bat kiln list kiln daily output up to 1.5 tons or more, the dou-ble-pusher kiln list kiln daily output is reachable
3.0 tons or more, substantially increase yield.
Specific embodiment
The present invention is described further below with reference to embodiment；
Embodiment 1:
Vanadium nitride yield and product quality are improved using following processing step:
(1) ingredient: 1 ton of vanadium trioxide and 280Kg graphite powder are mixed and be incorporated iron powder 8kg and makees additive；
(2) it charges: green-ball is fitted into the square stock tank and circle batch can for mixing and being launched in producing line in 2:1 ratio；
(3) reduction nitridation: after batch can enters kiln, successively by each warm area in kiln, each warm area temperature, 6 warm areas are controlled respectively
1000 DEG C, 1100 DEG C of 7 warm area, 1300 DEG C of 8 warm area, 1450 DEG C of 9 warm area, 1520 DEG C of 10-17 warm area；Control is passed through the flow of nitrogen
For 1-5 warm area 3600L/min, 6-8 warm area 5300L/min, 9 warm area nitrogen flows are 6300L/min, 10 warm areas and later nitrogen
Flow is 7000 L/min；Control kiln hood pressure 4Pa, pressure 10Pa, kiln tail pressure 14Pa in kiln；It is reacted under the conditions of high temperature nitrogen
14h obtains high yield, high quality vanadium nitride.Product apparently has metallic luster and flawless, apparent density 3.53g/cm3, single kiln
1.58 tons of daily output, product nitrogen content 15.63% entirely reaches VN16 standard.
Embodiment 2:
Vanadium nitride yield and product quality are improved using following processing step:
(1) ingredient: 1 ton of vanadium trioxide and 275Kg graphite powder are mixed and be incorporated iron powder 10kg and makees additive；
(2) it charges: green-ball is fitted into the square stock tank and circle batch can for mixing and being launched in producing line in 3:1 ratio；
(3) reduction nitridation: after batch can enters kiln, successively by each warm area in kiln, each warm area temperature, 6 warm areas are controlled respectively
1100 DEG C, 1200 DEG C of 7 warm area, 1350 DEG C of 8 warm area, 1450 DEG C of 9 warm area, 1530 DEG C of 10-17 warm area；Control is passed through the flow of nitrogen
For 1-5 warm area 3800L/min, 6-8 warm area 5500L/min, 9 warm area nitrogen flows are 6300L/min, 10 warm areas and later nitrogen
Flow is 7500 L/min；Control kiln hood pressure 6Pa, pressure 15Pa, kiln tail pressure 16Pa in kiln；It is reacted under the conditions of high temperature nitrogen
15h obtains high yield, high quality vanadium nitride.Product apparently has metallic luster and flawless, apparent density 3.58g/cm3, single kiln
1.63 tons of daily output, product nitrogen content 15.42% entirely reaches VN16 standard.
Embodiment 3:
Vanadium nitride yield and product quality are improved using following processing step:
(1) ingredient: 1 ton of vanadic anhydride and 350Kg graphite powder are mixed and be incorporated iron powder 6kg and makees additive；
(2) it charges: green-ball is fitted into the square stock tank and circle batch can for mixing and being launched in producing line in 1:1 ratio；
(3) reduction nitridation: after batch can enters kiln, successively by each warm area in kiln, each warm area temperature, 6 warm areas are controlled respectively
1000 DEG C, 1100 DEG C of 7 warm area, 1200 DEG C of 8 warm area, 1400 DEG C of 9 warm area, 1510 DEG C of 10-17 warm area；Control is passed through the flow of nitrogen
For 1-5 warm area 3500L/min, 6-8 warm area 5000L/min, 9 warm area nitrogen flows are 6000L/min, 10 warm areas and later nitrogen
Flow is 6500 L/min；Control kiln hood pressure 10Pa, pressure 20Pa, kiln tail pressure 8Pa in kiln；It is reacted under the conditions of high temperature nitrogen
13h obtains high yield, high quality vanadium nitride.Product apparently has metallic luster and flawless, apparent density 3.5g/cm3, single kiln
1.5 tons of daily output, product nitrogen content 14.45% entirely reaches VN16 standard.
Embodiment 4:
Vanadium nitride yield and product quality are improved using following processing step:
(1) ingredient: 1 ton of vanadic anhydride and 355Kg graphite powder are mixed and be incorporated iron powder 12kg and makees additive；
(2) it charges: green-ball is fitted into the square stock tank and circle batch can for mixing and being launched in producing line in 4:1 ratio；
(3) reduction nitridation: after batch can enters kiln, successively by each warm area in kiln, each warm area temperature, 6 warm areas are controlled respectively
1100 DEG C, 1200 DEG C of 7 warm area, 1350 DEG C of 8 warm area, 1500 DEG C of 9 warm area, 1540 DEG C of 10-17 warm area；Control is passed through the flow of nitrogen
For 1-5 warm area 4000L/min, 6-8 warm area 5800L/min, 9 warm area nitrogen flows are 6500L/min, 10 warm areas and later nitrogen
Flow is 8000 L/min；Control kiln hood pressure 1Pa, pressure 5Pa, kiln tail pressure 20Pa in kiln；Obtain high yield, high quality nitrogen
Change vanadium.Product apparently has metallic luster and flawless, apparent density 3.62g/cm3, single 1.72 tons of kiln daily output, product nitrogen content
14.12%, entirely reach VN16 standard.
Embodiment 5
Vanadium nitride yield and product quality are improved using following processing step:
(1) ingredient: 1 ton of vanadium trioxide and 280Kg graphite powder are mixed and be incorporated iron powder 7kg and makees additive；
(2) it charges: green-ball is fitted into the square stock tank and circle batch can for mixing and being launched in producing line in 2:1 ratio；
(3) reduction nitridation: after batch can enters kiln, successively by each warm area in kiln, each warm area temperature, 6 warm areas are controlled respectively
1050 DEG C, 1300 DEG C of 7 warm area, 1350 DEG C of 8 warm area, 1500 DEG C of 9 warm area, 1520 DEG C of 10-17 warm area；Control is passed through the flow of nitrogen
For 1-5 warm area 3800L/min, 6-8 warm area 5400L/min, 9 warm area nitrogen flows are 6500L/min, 10 warm areas and later nitrogen
Flow is 6500 L/min；Control kiln hood pressure 5Pa, pressure 18Pa, kiln tail pressure 10Pa in kiln；It is reacted under the conditions of high temperature nitrogen
15h obtains high yield, high quality vanadium nitride.Product apparently has metallic luster and flawless, apparent density 3.58g/cm3, single kiln
1.70 tons of daily output, product nitrogen content 14.15% entirely reaches VN16 standard.
Embodiment 6
Vanadium nitride yield and product quality are improved using following processing step:
(1) ingredient: 1 ton of vanadium trioxide and 275Kg graphite powder are mixed and be incorporated iron powder 11kg and makees additive；
(2) it charges: green-ball is fitted into the square stock tank and circle batch can for mixing and being launched in producing line in 3:1 ratio；
(3) reduction nitridation: after batch can enters kiln, successively by each warm area in kiln, each warm area temperature, 6 warm areas are controlled respectively
1080 DEG C, 1250 DEG C of 7 warm area, 1300 DEG C of 8 warm area, 1450 DEG C of 9 warm area, 1540 DEG C of 10-17 warm area；Control is passed through the flow of nitrogen
For 1-5 warm area 4000L/min, 6-8 warm area 5600L/min, 9 warm area nitrogen flows are 6400L/min, 10 warm areas and later nitrogen
Flow is 7800 L/min；Control kiln hood pressure 8Pa, pressure 8Pa, kiln tail pressure 18Pa in kiln；It is reacted under the conditions of high temperature nitrogen
13h obtains high yield, high quality vanadium nitride.Product apparently has metallic luster and flawless, apparent density 3.61g/cm3, single kiln
1.73 tons of daily output, product nitrogen content 14.13% entirely reaches VN16 standard.
Comparative example 1:
Except ingredient is added in addition to iron powder amount is 1kg in this comparative example, other batch cans launch ratio and technology controlling and process with implementation
Example 1 is identical, and product apparently without metallic luster and has crackle, apparent density 3.42g/cm3, single 1.51 tons of kiln daily output, product is nitrogenous
Amount 15.42%, entirely reaches VN16 standard.
Comparative example 2:
Except ingredient is added in addition to iron powder amount is 15kg in this comparative example, other batch cans launch ratio and technology controlling and process with implementation
Example 1 is identical, and product apparently has metallic luster and flawless, apparent density 3.7g/cm3, single kiln daily output is up to 1.61 tons, but product
Containing vanadium 76.87, it is lower than national standard, product is unqualified.
Comparative example 3:
In this comparative example in addition to square stock tank and circle batch can launch ratio only to launch circle batch can, ingredient and other technology controlling and process
Same as Example 1, product apparently has metallic luster and flawless, apparent density 3.51g/cm3, single 1.43 tons of kiln daily output,
Product nitrogen content 14.77%, entirely reaches VN16 standard, and yield and nitrogen content decrease.
Comparative example 4:
In this comparative example in addition to square stock tank and circle batch can launch ratio only to launch square stock tank, ingredient and other technology controlling and process
Same as Example 1, product apparently has metallic luster and flawless, apparent density 3.51g/cm3, single 1.69 tons of kiln daily output,
Product nitrogen content 14.06% entirely reaches VN16 standard, and yield greatly improves but product nitrogen content is greatly reduced, product quality drop
It is low larger.
Comparative example 5:
750 DEG C of 6 warm area, 950 DEG C of 7 warm area, 1100 DEG C of 8 warm area, 1200 DEG C of 9 warm area, 10 warm areas 1350 are removed in this comparative example
DEG C, 1450 DEG C of 11 warm area (i.e. high-temperature region is since 12 warm areas) outside, ingredient, batch can launch ratio and other technology controlling and process with reality
It is identical to apply example 1, product apparently has metallic luster and flawless, apparent density 3.22g/cm3, single 1.51 tons of kiln daily output, product contains
Nitrogen quantity 13.2% is VN12, and product nitrogen content and apparent density decline to a great extent.
Comparative example 6:
Increase low-temperature space nitrogen flow except 1-5 warm area nitrogen flow becomes 5500L/min(in this comparative example) in addition to, match
Material, batch can launch ratio and other technology controlling and process are same as Example 1, and product apparently has metallic luster and flawless, apparently
Density 3.52g/cm3, single 1.51 tons of kiln daily output, product nitrogen content 15.01% entirely reaches VN16 standard, but since exhaust gas is discharged
Nitridation is influenced not in time, and product nitrogen content is declined slightly.
Comparative example 7:
High temperature and later warm area nitrogen are reduced except the later nitrogen flow of 10 warm areas becomes 5500L/min(i.e. in this comparative example
Flow) outside, ingredient, batch can launch ratio and other technology controlling and process are same as Example 1, and product apparently has metallic luster and nothing
Crackle, apparent density 3.52g/cm3, single 1.51 tons of kiln daily output, product nitrogen content 14.23% entirely reaches VN16 standard, but produces
Product nitrogen content declines to a great extent.
Comparative example 8:
Control kiln hood pressure 14Pa, pressure 40Pa, kiln tail pressure 34Pa in kiln, remaining ingredient, batch can are removed in this comparative example
Dispensing ratio and other technology controlling and process are same as Example 1, and product apparently has metallic luster and flawless, apparent density
3.52g/cm3, single kiln produces 1.51 tons daily, product nitrogen content 12.53%, product VN12, and product nitrogen content declines to a great extent, seriously
Influence product quality.
Comparative example 9:
Except kiln hood pressure 1Pa, pressure 1Pa in kiln, kiln tail pressure 1Pa is controlled in this comparative example, remaining ingredient, batch can are launched
Ratio and other technology controlling and process are same as Example 1, and product apparently has metallic luster and flawless, but has oxidative phenomena, table
See density 3.52g/cm3, single kiln produces 1.51 tons daily, product nitrogen content 12.75%, product VN12, product nitrogen content substantially under
Drop, seriously affects product quality.
Integrated embodiment 1-6 and comparative example 1-9 result can be seen that the present invention and substantially increase pushed bat kiln yield, and energy
The nitrogen content and apparent density for enough improving vanadium nitride reduce product crackle and product are made to show metallic luster, to improve
The quality of vanadium nitride.
It is defined in the present invention and iron powder amount is added to 6-12kg/ tons of barium oxides, crossed low energy and produce qualified products but table
Appearance quality is poor, excessively high, easily causes product unqualified；The side of defining, the dispensing ratio for justifying batch can are 1:1 ~ 4:1, do not put square stock tank
Or square stock tank excessively all can be because of product nitrogen content reduction caused by nitrogen irrational distribution；And shift to an earlier date high temperature area, control 6 warm areas
1000 DEG C -1100 DEG C of temperature；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 product is nitrogenous to be promoted by VN12 at 1510 DEG C -1540 DEG C in the case where load is constant
To VN16 standard；And it is 3500-4000 L/min that nitrogen flow, which is set as 1-5 warm area nitrogen flow,；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, further preferably 1-5 warm area nitrogen flow are 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
When L/min, product nitrogen content is higher, and increasing or reducing nitrogen flow will cause the reduction of product nitrogen content；And pressure control kiln
Head pressure 1-10Pa, pressure 5-20Pa in kiln, kiln tail pressure 8-20Pa is further preferred are as follows: kiln hood pressure 4-6Pa, pressure in kiln
After 10-15Pa, kiln tail pressure 14-16Pa, the nitrogenous height of product, and furnace pressure is increased or reduced, it will cause the declines of product nitrogen content
Until there is VN12 product；
Therefore vanadium nitride is produced using this technology pushed bat kiln, pushed bat kiln yield, single pushed bat kiln list kiln day can be effectively increased
Yield is up to 1.5 tons or more, and the dou-ble-pusher kiln list kiln daily output is up to 3.0 tons or more；And the apparent flawless of product can be made, it is in metal
Gloss, apparent density reach 3.5g/cm3More than, all VN16 of product.
Method detailed of the invention that the present invention is explained by the above embodiments, but the invention is not limited to it is above-mentioned in detail
Method, that is, do not mean that the invention must rely on the above detailed methods to implement.Person of ordinary skill in the field should
It is illustrated, any improvement in the present invention, addition, the concrete mode of equivalence replacement and auxiliary element to each raw material of product of the present invention
Selection etc., all of which fall within the scope of protection and disclosure of the present invention.
Claims (6)
1. a kind of method of pushed bat kiln production vanadium nitride, it is characterised in that: include the following steps:
(1) excess iron powder is added when ingredient, the iron powder amount of addition is 7-10kg/ tons of vanadium trioxide meters；
(2) it charges: charging method is mixed using square stock tank and circle batch can, green-ball is packed into mixing in proportion and is launched in producing line
In square stock tank and circle batch can；
(3) reduction nitridation: after batch can enters kiln, successively by each warm area in kiln, each warm area temperature is controlled respectively and is passed through nitrogen
Flow, and the furnace chamber pressure in kiln hood, kiln and at kiln tail is controlled, it is reacted under a nitrogen atmosphere, obtains vanadium nitride
Product；Temperature control is 1000 DEG C -1100 DEG C of 6 warm area；1100 DEG C -1350 DEG C of 7-8 warm area；9 1400 DEG C -1500 DEG C of warm areas；10-
17 1510 DEG C -1540 DEG C of warm areas；The nitrogen flow control that each warm area is passed through are as follows: 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.
2. a kind of method of pushed bat kiln production vanadium nitride according to claim 1, it is characterised in that side in the step (2)
It is 1:1-4:1 that batch can, which mixes the ratio launched in producing line with circle batch can,.
3. a kind of method of pushed bat kiln production vanadium nitride according to claim 2, it is characterised in that side in the step (2)
It is 2:1 or 3:1 that batch can and circle batch can, which launch ratio,.
4. a kind of method of pushed bat kiln production vanadium nitride according to claim 1, it is characterised in that each in the step (3)
The nitrogen flow control that warm area is passed through are as follows: 3600 L/min -3800 L/min of 1-5 warm area；6-8 warm area 5300-5500 L/
min；9 warm area 6300L/min, 10 warm areas and later 7000-7500 L/min.
5. a kind of method of pushed bat kiln production vanadium nitride according to claim 1, it is characterised in that kiln in the step (3)
Voltage-controlled to be made as: kiln hood pressure 1-10Pa, pressure 5-20Pa in kiln, kiln tail pressure 8-20Pa, condition of nitrogen gas lower reaction time are 13-
15h。
6. a kind of method of pushed bat kiln production vanadium nitride according to claim 5, it is characterised in that kiln in the step (3)
It is voltage-controlled to be made as: kiln hood pressure 4-6Pa, pressure 10-15Pa, kiln tail pressure 14-16Pa in kiln.
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| CN101289713A (en) * | 2007-04-20 | 2008-10-22 | 郸城财鑫特种金属有限责任公司 | Production process of vanadium-nitrogen alloy |
| CN102173395A (en) * | 2011-01-05 | 2011-09-07 | 武安市炜荣物资有限公司 | Simple vanadium nitride production method |
| CN102910596A (en) * | 2012-08-16 | 2013-02-06 | 中色（宁夏）东方集团有限公司 | Preparation method of vanadium nitride |
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| CN101289713A (en) * | 2007-04-20 | 2008-10-22 | 郸城财鑫特种金属有限责任公司 | Production process of vanadium-nitrogen alloy |
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| CN102910596A (en) * | 2012-08-16 | 2013-02-06 | 中色（宁夏）东方集团有限公司 | Preparation method of vanadium nitride |
| CN104004958A (en) * | 2014-06-16 | 2014-08-27 | 四川展祥特种合金科技有限公司 | Method and device for continuously preparing vanadium-nitrogen alloy |
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