CN108004403A - A kind of rotary kiln vanadium nitrogen alloy preparation method and equipment - Google Patents

A kind of rotary kiln vanadium nitrogen alloy preparation method and equipment Download PDF

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Publication number
CN108004403A
CN108004403A CN201711307889.8A CN201711307889A CN108004403A CN 108004403 A CN108004403 A CN 108004403A CN 201711307889 A CN201711307889 A CN 201711307889A CN 108004403 A CN108004403 A CN 108004403A
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CN
China
Prior art keywords
rotary kiln
input terminal
electrode input
negative electrode
positive electrode
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CN201711307889.8A
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Chinese (zh)
Inventor
叶晓林
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Sichuan Zhongyi Control Industrial Development Co Ltd
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Sichuan Zhongyi Control Industrial Development Co Ltd
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Priority to CN201711307889.8A priority Critical patent/CN108004403A/en
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B4/00Electrothermal treatment of ores or metallurgical products for obtaining metals or alloys
    • C22B4/06Alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B4/00Electrothermal treatment of ores or metallurgical products for obtaining metals or alloys
    • C22B4/08Apparatus

Abstract

The invention discloses a kind of rotary kiln vanadium nitrogen alloy preparation method, including crush milling, raw material mixing, curing catalysis, compound stalk forming and reduction nitridation;A kind of rotary kiln VN alloy production equipment, including rotary kiln, positive electrode input terminal and negative electrode input terminal, positive electrode input terminal are arranged at the feed inlet of rotary kiln, and negative electrode input terminal is arranged on the discharge outlet of rotary kiln;Compound containing vanadium and oxygen, organic carbon or inorganic carbon and additive are mixed to form raw material by a kind of rotary kiln vanadium nitrogen alloy preparation method of the present invention and equipment, then being directly powered in electrically direct-heating rotary kiln to raw material makes it generate heat and is progressively warming up to more than 1150 DEG C, reduction nitridation generates VN alloy, its heat source produces raw material resistance heating from externally fed, the thermal efficiency is high, power consumption is low, process stabilizing.

Description

A kind of rotary kiln vanadium nitrogen alloy preparation method and equipment
Technical field
The present invention relates to the production of VN alloy, more particularly to a kind of rotary kiln vanadium nitrogen alloy preparation method and equipment.
Background technology
VN alloy is a kind of novel alloy additive, can substitute the production that vanadium iron is used for micro alloyed steel.Vanadium nitride The comprehensive mechanical performances such as intensity, toughness, ductility and the thermal fatigue resistance of steel can be improved by making an addition in steel, and it is good to have steel Solderability.The production method of the VN alloy possessed now is likely to occur the feelings that the efficiency of heating surface is low, power consumption is high, technique is unstable Condition.
The content of the invention
The purpose of the present invention be that provide to solve the above-mentioned problems a kind of rotary kiln vanadium nitrogen alloy preparation method and Equipment.
The present invention is achieved through the following technical solutions above-mentioned purpose:
A kind of rotary kiln vanadium nitrogen alloy preparation method, comprises the following steps:
S1, crush milling, oxyvanadium compound is carried out crushing milling, milling granularity is more than 150 mesh;
S2, raw material mixing, oxyvanadium compound powder, carbon dust and material catalytic additive are added in 0.5% ratio and stirred Mix machine uniformly to mix, its physical catalyst is iron oxide mixture;
S3, curing catalysis, add clear water to mixed material, are warming up to 80 DEG C~120 DEG C, further roll mixing, mix After the completion of, raw material is put into batch can, stands catalysis, standing time is more than 24h;
S4, compound stalk forming, send the raw material after catalysis into forming machine, are pressed into the sphere of a diameter of 5cm, spontaneously dry 48h;
S5, reduction nitridation, send dried raw material into rotary kiln, are passed through nitrogen to rotary kiln, are reacted it, walk It is rapid as follows:
A1, drying and dehydrating, by material be sent into rotary kiln pre-reaction zone, control pre-reaction zone temperature be maintained at 150 DEG C~ 200 DEG C, soaking time 2h;
A2, vanadium nitrogen pre-reaction, pre-reaction zone of heating up, temperature are remained as 550 DEG C~650 DEG C, run time 4h~6h;
A3, pyroreaction, send material into main reaction region, material is added with the rate of heat addition of 12 DEG C/min~15 DEG C/min Hot to 1350 DEG C~1550 DEG C, reaction time 6h~8h;
A4, cooling discharging, send material into cooling zone, and keep positive pressure of nitrogen state, cool down 4h~6h, and temperature is less than Lower stove after 100 DEG C.
Specifically, in above-mentioned steps S5, the air pressure in rotary kiln is the barotropic state less than 5MPa.
A kind of rotary kiln VN alloy production equipment, including rotary kiln, positive electrode input terminal and negative electrode input terminal, it is described Positive electrode input terminal is arranged at the feed inlet of the rotary kiln, and the negative electrode input terminal is arranged on the discharging of the rotary kiln At mouthful, the inner of the positive electrode input terminal is arranged in the rotary kiln, and the inner of the negative electrode input terminal is arranged on institute State in rotary kiln, the inner and described negative electrode input terminal of the positive electrode input terminal it is inner with the thing in the rotary kiln Material contact, the outer end of the outer end of the positive electrode input terminal and the negative electrode input terminal is respectively with the cathode of DC power supply and bearing Pole is electrically connected;
Be pre-reaction zone between the feed inlet and the positive electrode input terminal, for material is dried with it is pre- anti- Should;
It is main reaction region between the positive electrode input terminal and the negative electrode input terminal, for material and nitrogen progress Reaction;
It is cooling zone between the negative electrode input terminal and the discharge port, for cooling down the material after reacting.
The beneficial effects of the present invention are:
A kind of rotary kiln vanadium nitrogen alloy preparation method of the present invention and equipment are by the compound containing vanadium and oxygen, organic carbon or nothing Machine carbon is mixed to form raw material with additive, and being then directly powered in electrically direct-heating rotary kiln to raw material makes it generate heat and progressively rise For temperature to more than 1150 DEG C, reduction nitridation generation VN alloy, its heat source produces raw material resistance heating, the thermal efficiency from externally fed Height, power consumption is low, process stabilizing.
Embodiment
The invention will be further described below:
A kind of rotary kiln vanadium nitrogen alloy preparation method of the present invention, including crush milling, raw material mixing, curing catalysis, briquetting Shaping and reduction nitridation, specially carry out crushing milling by oxyvanadium compound, and milling granularity is more than 150 mesh;By oxyvanadium compound Powder, carbon dust and material catalytic additive add mixer in 0.5% ratio and uniformly mix, its physical catalyst is iron oxide Mixture;Clear water is added to mixed material, 80 DEG C~120 DEG C is warming up to, further rolls mixing, after the completion of mixing, by raw material Batch can is put into, stands catalysis, standing time is more than 24h;Raw material after catalysis is sent into forming machine, is pressed into a diameter of 5cm's Sphere, spontaneously dries 48h;Dried raw material is sent into rotary kiln, nitrogen is passed through to rotary kiln, and including in rotary kiln Air pressure is reacted it for the barotropic state less than 5MPa.
Its reduction nitridation reaction specifically includes:Drying and dehydrating, the pre-reaction of vanadium nitrogen, pyroreaction and cooling are come out of the stove;
Material is sent into the pre-reaction zone of rotary kiln, control pre-reaction zone temperature is maintained at 150 DEG C~200 DEG C, during insulation Between 2h;After treatment, furnace charge moisture content drops to less than 0.2%.
Heat up pre-reaction zone, temperature is remained as 550 DEG C~650 DEG C, run time 4h~6h;In the molten of high price vanadium oxide Under point, controlling generation low price vanadium nitride, reduces vanadium oxide loss.
Material is sent into main reaction region, material is heated to 1350 DEG C with the rate of heat addition of 12 DEG C/min~15 DEG C/min ~1550 DEG C, reaction time 6h~8h;Material enters main reaction region from electrode input end, and vanadium raw materials are by pre- in heating process Reduction process and reduction nitridation process in nitriding atmosphere and synthesize VN alloy, produce vanadium-nitrogen alloy product.
Cooling discharging, send material into cooling zone, to prevent VN alloy secondary oxidation, keeps positive pressure of nitrogen state, cold But 4h~6h, temperature lower stove after being less than 100 DEG C.
A kind of rotary kiln VN alloy production equipment, including rotary kiln, positive electrode input terminal and negative electrode input terminal, positive electricity Pole input terminal is arranged at the feed inlet of rotary kiln, and negative electrode input terminal is arranged on the discharge outlet of rotary kiln, positive electrode input The inner at end is arranged in rotary kiln, and the inner of negative electrode input terminal is arranged in rotary kiln, positive electrode input terminal the inner and The inner of negative electrode input terminal is contacted with the material in rotary kiln, the outer end of positive electrode input terminal and negative electrode input terminal it is outer End is electrically connected with the cathode and anode of DC power supply respectively;Be pre-reaction zone between feed inlet and positive electrode input terminal, for pair Material is dried and pre-reaction;It is main reaction region between positive electrode input terminal and negative electrode input terminal, for material and nitrogen Gas is reacted;It is cooling zone between negative electrode input terminal and discharge port, for cooling down the material after reacting.
Oxyvanadium compound passes through solid of the DC power supply electrode pair containing vanadium and carbonaceous reducing agent in electrical heating rotary kiln Raw material (ball is block) direct-electrifying, is generated heat by the contact resistance between the resistance or raw material ellipsoid bulk of solid material itself And solid material is heated, the thermal efficiency is high, and power consumption is low, process stabilizing.
Technical scheme is not limited to the limitation of above-mentioned specific embodiment, and every technique according to the invention scheme is done The technology deformation gone out, each falls within protection scope of the present invention.

Claims (3)

1. a kind of rotary kiln vanadium nitrogen alloy preparation method, it is characterised in that comprise the following steps:
S1, crush milling, oxyvanadium compound is carried out crushing milling, milling granularity is more than 150 mesh;
S2, raw material mixing, mixer is added by oxyvanadium compound powder, carbon dust and material catalytic additive in 0.5% ratio Uniformly mixing, its physical catalyst is iron oxide mixture;
S3, curing catalysis, add clear water to mixed material, are warming up to 80 DEG C~120 DEG C, further roll mixing, and mixing is completed Afterwards, raw material is put into batch can, stands catalysis, standing time is more than 24h;
S4, compound stalk forming, send the raw material after catalysis into forming machine, are pressed into the sphere of a diameter of 5cm, spontaneously dry 48h;
S5, reduction nitridation, send dried raw material into rotary kiln, are passed through nitrogen to rotary kiln, are reacted it, step is such as Under:
Material, is sent into the pre-reaction zone of rotary kiln by A1, drying and dehydrating, and control pre-reaction zone temperature is maintained at 150 DEG C~200 DEG C, soaking time 2h;
A2, vanadium nitrogen pre-reaction, pre-reaction zone of heating up, temperature are remained as 550 DEG C~650 DEG C, run time 4h~6h;
A3, pyroreaction, send material into main reaction region, material is heated to the rate of heat addition of 12 DEG C/min~15 DEG C/min 1350 DEG C~1550 DEG C, reaction time 6h~8h;
A4, cooling discharging, send material into cooling zone, and keep positive pressure of nitrogen state, cool down 4h~6h, and temperature is less than 100 DEG C Stove is descended afterwards.
A kind of 2. rotary kiln vanadium nitrogen alloy preparation method according to claim 1, it is characterised in that:In above-mentioned steps S5, Air pressure in rotary kiln is the barotropic state less than 5MPa.
A kind of 3. rotary kiln VN alloy production equipment, it is characterised in that:It is defeated including rotary kiln, positive electrode input terminal and negative electrode Enter end, the positive electrode input terminal is arranged at the feed inlet of the rotary kiln, and the negative electrode input terminal is arranged on the rotation The discharge outlet of rotary kiln, the inner of the positive electrode input terminal are arranged in the rotary kiln, the negative electrode input terminal it is interior End be arranged in the rotary kiln, the inner and described negative electrode input terminal of the positive electrode input terminal the inner with the rotation Material contact in rotary kiln, the outer end of the outer end of the positive electrode input terminal and the negative electrode input terminal respectively with DC power supply Cathode and anode be electrically connected;
It is pre-reaction zone between the feed inlet and the positive electrode input terminal, for material being dried and pre-reaction;
It is main reaction region between the positive electrode input terminal and the negative electrode input terminal, it is anti-for being carried out to material and nitrogen Should;
It is cooling zone between the negative electrode input terminal and the discharge port, for cooling down the material after reacting.
CN201711307889.8A 2017-12-11 2017-12-11 A kind of rotary kiln vanadium nitrogen alloy preparation method and equipment Pending CN108004403A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108963280A (en) * 2018-07-11 2018-12-07 武汉科技大学 The method for preparing carbon-based elctro-catalyst is pyrolyzed based on Joule heat

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101717883A (en) * 2009-07-22 2010-06-02 隋智通 Continuous production method of vanadium (iron) carbonitride and device thereof
CN101921941A (en) * 2010-09-17 2010-12-22 甘锦旺 Method for producing vanadium-nitrogen alloy
CN103335513A (en) * 2012-12-10 2013-10-02 冯良荣 Electric heating rotary kiln
CN103466569A (en) * 2009-10-12 2013-12-25 冯良荣 Method for preparing vanadium nitride
CN204007095U (en) * 2014-07-15 2014-12-10 机械工业第六设计研究院有限公司 High-accuracy electric heating nitriding furnace
CN105483507A (en) * 2016-01-05 2016-04-13 北京科技大学 Nitrided ferrovanadium alloy and preparing method thereof
CN105838959A (en) * 2016-05-31 2016-08-10 九江市钒宇新材料有限公司 Vanadium nitrogen microalloy additive and preparing method thereof

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101717883A (en) * 2009-07-22 2010-06-02 隋智通 Continuous production method of vanadium (iron) carbonitride and device thereof
CN103466569A (en) * 2009-10-12 2013-12-25 冯良荣 Method for preparing vanadium nitride
CN101921941A (en) * 2010-09-17 2010-12-22 甘锦旺 Method for producing vanadium-nitrogen alloy
CN103335513A (en) * 2012-12-10 2013-10-02 冯良荣 Electric heating rotary kiln
CN204007095U (en) * 2014-07-15 2014-12-10 机械工业第六设计研究院有限公司 High-accuracy electric heating nitriding furnace
CN105483507A (en) * 2016-01-05 2016-04-13 北京科技大学 Nitrided ferrovanadium alloy and preparing method thereof
CN105838959A (en) * 2016-05-31 2016-08-10 九江市钒宇新材料有限公司 Vanadium nitrogen microalloy additive and preparing method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108963280A (en) * 2018-07-11 2018-12-07 武汉科技大学 The method for preparing carbon-based elctro-catalyst is pyrolyzed based on Joule heat

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Application publication date: 20180508

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