CN104531999A - Method for preparing vanadium-nitrogen alloy - Google Patents

Method for preparing vanadium-nitrogen alloy Download PDF

Info

Publication number
CN104531999A
CN104531999A CN201510001232.3A CN201510001232A CN104531999A CN 104531999 A CN104531999 A CN 104531999A CN 201510001232 A CN201510001232 A CN 201510001232A CN 104531999 A CN104531999 A CN 104531999A
Authority
CN
China
Prior art keywords
vanadium
alloy
sintering
iron powder
temperature
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201510001232.3A
Other languages
Chinese (zh)
Inventor
葛广凯
戴红梅
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nantong Hanrui Industrial Co Ltd
Original Assignee
Nantong Hanrui Industrial Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Nantong Hanrui Industrial Co Ltd filed Critical Nantong Hanrui Industrial Co Ltd
Priority to CN201510001232.3A priority Critical patent/CN104531999A/en
Publication of CN104531999A publication Critical patent/CN104531999A/en
Pending legal-status Critical Current

Links

Abstract

The invention provides a method for preparing vanadium-nitrogen alloy. The method comprises the steps that vanadium oxide, graphite powder and a catalyst are evenly mixed, and the mixed materials are compressed to be spherical or elliptical raw materials; afterwards, the raw materials are placed in a sintering furnace full of nitrogen to be sintered, and the vanadium-nitrogen alloy can be obtained after sintering is completed; the catalyst is iron powder; the sintering process of the sintering furnace is that the temperature is made to rise to 1300-1500 DEG C, which is the highest temperature, within six hours; the vanadium oxide comprises at least one of vanadium pentoxide, vanadium tetraoxide and vanadium trioxide.

Description

A kind of preparation method of VN alloy
Technical field
The present invention relates to the preparation field of chemical materials, especially design utilizes iron powder as the method for catalyst preparing VN alloy.
Background technology
VN alloy is a kind of Novel steel iron additive, the method of current production VN alloy is that vanadium oxide (mixtures of Vanadium Pentoxide in FLAKES, vanadium tetraoxide, vanadous oxide or three kinds) adds reductive agent graphite briquetting, what utilize powder metallurgy is placed in high temperature nitrogen atmosphere, generates VN alloy by reduction, nitrogenizing reaction.Determine its reduction by the character of vanadium, nitrogenizing reaction theoretical temperatures must higher than 1250 DEG C, general in order to production efficiency in production, general temperature is more than 1600 DEG C, and too high temperature result in higher energy consumption, refractory wear, also high to equipment requirements.In the production method of a kind of VN alloy provided as Chinese patent (CN103243254A), first being reduced into by Vanadium Pentoxide in FLAKES is vanadium tetraoxide, then add carbon dust to carry out segmentation again and react, but require that nitrogen passes into the certain malleation of rear maintenance, simultaneous temperature rises to 1500 ~ 1600 DEG C, and this production method is also higher to equipment requirements.
The preparation technology of the low VN alloy of current scholar both domestic and external promotes, wherein, Chinese patent (CN 2102277522A) provides a kind of method of producing VN alloy, adopt vanadium raw materials, additive, C matter reductive agent and binding agent are as reaction raw materials, wherein additive is ferric oxide, the ferro element materials such as Z 250, vanadium raw materials selects ammonium meta-vanadate, poly ammonium vanadate and Vanadium Pentoxide in FLAKES etc., but in this production method, adopt Vanadium Pentoxide in FLAKES, vanadium tetraoxide, when vanadous oxide or three's mixture, the yield of reaction product is lower, after adding binding agent simultaneously, yield rise to some extent but the appearance in final product from the impurity of binding agent, affect final purity, in addition, during high temperature sintering when directly directly being carried out by the dried material after shaping, there will be product caking or over-reactive problem.In sum, in the method for current technology production VN alloy, there is synthetic technology interalloy purity or the poor problem of yield, also comprise the higher temperature of reaction of production method and the time requires high problem to conversion unit.
Summary of the invention
The present invention proposes a kind of preparation method of VN alloy, adopts iron powder as catalyzer and the reactive mode that progressively heats up, solve in prior art to vanadium oxide be raw material prepare VN alloy time production yield and the lower problem of purity.
Technical scheme of the present invention is achieved in that
A preparation method for VN alloy, step is as follows: vanadium oxide, Graphite Powder 99 and catalyst mix is even, compound is pressed into spherical or ellipticity raw material; Subsequently, inserting in the sintering oven being full of nitrogen of raw material is sintered, after terminating, namely obtains product; Described catalyzer is iron powder; The sintering process of described sintering oven is: temperature is raised to top temperature 1300 ~ 1500 DEG C for 6 hours; Described vanadium oxide is at least one in Vanadium Pentoxide in FLAKES, vanadium tetraoxide, vanadous oxide.
Wherein, preferably, described iron powder accounts for the ratio of gross weight and is: 0.3% ~ 1.5%.Further preferably, the ratio that described iron powder accounts for gross weight is 1.2%.
Further preferably, when the carrying out of described sintering oven sinters, under top temperature, be incubated 2 ~ 4 hours.
In the application, using vanadium oxide (Vanadium Pentoxide in FLAKES, vanadium tetraoxide, vanadous oxide) supplying raw materials as main v element, first vanadium oxide is reduced during reaction, carry out the replacement of oxygen element, adopt iron powder as catalyzer, just because of iron powder can form ferric oxide in sintering or reaction process, when can improve whole reaction, the speed that is reduced of vanadium oxide, also reduces reduction temperature simultaneously; Ferro element is to the affinity of nitrogen higher than v element in addition, effectively reduces the temperature of overall reduction and nitrogenize in sintering process, also the corresponding speed that improve reduction and nitrogenize.Reduction temperature is reduced to 1400 DEG C; Simultaneously during pyroreaction, adopt the mode that progressively temperature raising react, when tentatively reducing, can ensure that iron powder is in the process forming ferric oxide, reduce selecting of over-reactive problem and other catalyzer, the purity of raising VN alloy.In this preparation method, reduction nitridation temperature is reduced to 1400 DEG C from 1600 DEG C; High-temperature holding time dropped within 4 hours from 6 hours.
Embodiment
Below in conjunction with the embodiment of the present invention, be clearly and completely described technical scheme of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
In the VN alloy method that the present invention produces, step is as follows: vanadium oxide, Graphite Powder 99 and catalyst mix is even, compound is pressed into spherical or ellipticity raw material; Subsequently, inserting in the sintering oven being full of nitrogen of raw material is sintered, after terminating, namely obtains product; Described catalyzer is iron powder; The sintering process of described sintering oven is: temperature is raised to top temperature 1300 ~ 1500 DEG C for 6 hours; Described vanadium oxide is at least one in Vanadium Pentoxide in FLAKES, vanadium tetraoxide, vanadous oxide.
Wherein, be not limited to Graphite Powder 99 as reductive agent, also can be selected from gac, wood charcoal powder, refinery coke and coke etc.; Iron powder is the aggregates body that size is less than the iron of 1mm, and color is black, is pure metal iron.Pushed bat kiln is a kind of continous way heat-agglomerating equipment, can according to the processing requirement of sintered products, the continuous print warm area needed for layout and power; Owing to adopting Graphite Powder 99 as reductive agent, Graphite Powder 99 has sensitive chemical reactivity, there is good thermal conductivity simultaneously, and select iron powder as catalyzer, utilize pushed bat kiln to carry out temperature control during sintering, improve yield and the purity of whole reacting final product, and effectively reduce process temperature, reduce energy consumption, save cost.
Embodiment 1
By vanadium oxide (mixture of Vanadium Pentoxide in FLAKES, vanadium tetraoxide, vanadous oxide or three), Graphite Powder 99 and iron powder according to mixing evenly, wherein iron powder accounts for 0.3% of total mass.In ball press, pressing treatment is carried out to above-mentioned compound, obtain spherical raw material.Raw material are put into sintering oven, and sintering oven sintering process is: within 6 hours, be raised to 1300 DEG C by normal temperature, and is incubated 4 hours in the highest temperature; Ensure in sintering process to be full of nitrogen in stove.Sintering terminates, and after stove naturally cooling, namely product has sintered.Wherein, in the VN alloy finally obtained, the proportion of v element and nitrogen element is 98.9%, and other constituent contents are less.
Embodiment 2
By vanadium oxide (mixture of Vanadium Pentoxide in FLAKES, vanadium tetraoxide, vanadous oxide or three), Graphite Powder 99 and iron powder according to mixing evenly, wherein iron powder accounts for 1% of total mass.In ball press, pressing treatment is carried out to above-mentioned compound, obtain spherical raw material.Raw material are put into sintering oven, and sintering oven sintering process is: within 6 hours, be raised to 1400 DEG C by normal temperature, and is incubated 2 hours in the highest temperature; Ensure in sintering process to be full of nitrogen in stove.Sintering terminates, and after stove naturally cooling, namely product has sintered.Wherein, in the VN alloy finally obtained, the proportion of v element and nitrogen element is 98.8%, and other constituent contents are less.
Embodiment 3
By vanadium oxide (mixture of Vanadium Pentoxide in FLAKES, vanadium tetraoxide, vanadous oxide or three), Graphite Powder 99 and iron powder according to mixing evenly, wherein iron powder accounts for 0.8% of total mass.In ball press, pressing treatment is carried out to above-mentioned compound, obtain spherical raw material.Raw material are put into sintering oven, and sintering oven sintering process is: within 6 hours, be raised to 1500 DEG C by normal temperature, and is incubated 3 hours in the highest temperature; Ensure in sintering process to be full of nitrogen in stove.Sintering terminates, and after stove naturally cooling, namely product has sintered.Wherein, in the VN alloy finally obtained, the proportion of v element and nitrogen element is 99.0%, and other constituent contents are less.
Embodiment 4
By vanadium oxide (mixture of Vanadium Pentoxide in FLAKES, vanadium tetraoxide, vanadous oxide or three), Graphite Powder 99 and iron powder according to mixing evenly, wherein iron powder accounts for 1.5% of total mass.In ball press, pressing treatment is carried out to above-mentioned compound, obtain spherical raw material.Raw material are put into sintering oven, and sintering oven sintering process is: within 6 hours, be raised to 1500 DEG C by normal temperature, and is incubated 4 hours in the highest temperature; Ensure in sintering process to be full of nitrogen in stove.Sintering terminates, and after stove naturally cooling, namely product has sintered.Wherein, in the VN alloy finally obtained, the proportion of v element and nitrogen element is 99.1%, and other constituent contents are less.
Embodiment 5
By vanadium oxide (mixture of Vanadium Pentoxide in FLAKES, vanadium tetraoxide, vanadous oxide or three), Graphite Powder 99 and iron powder according to mixing evenly, wherein iron powder accounts for 1.4% of total mass.In ball press, pressing treatment is carried out to above-mentioned compound, obtain spherical raw material.Raw material are put into sintering oven, and sintering oven sintering process is: within 6 hours, be raised to 1250 DEG C by normal temperature, and is incubated 3 hours in the highest temperature; Ensure in sintering process to be full of nitrogen in stove.Sintering terminates, and after stove naturally cooling, namely product has sintered.Wherein, in the VN alloy finally obtained, the proportion of v element and nitrogen element is 99.0%, and other constituent contents are less.
Embodiment 46
By vanadium oxide (mixture of Vanadium Pentoxide in FLAKES, vanadium tetraoxide, vanadous oxide or three), Graphite Powder 99 and iron powder according to mixing evenly, wherein iron powder accounts for 0.8% of total mass.In ball press, pressing treatment is carried out to above-mentioned compound, obtain spherical raw material.Raw material are put into sintering oven, and sintering oven sintering process is: within 6 hours, be raised to 1400 DEG C by normal temperature, and is incubated 3 hours in the highest temperature; Ensure in sintering process to be full of nitrogen in stove.Sintering terminates, and after stove naturally cooling, namely product has sintered.Wherein, in the VN alloy finally obtained, the proportion of v element and nitrogen element is 98.8%, and other constituent contents are less.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.

Claims (4)

1. a preparation method for VN alloy, is characterized in that, step is as follows: vanadium oxide, Graphite Powder 99 and catalyst mix is even, compound is pressed into spherical or elliptoid raw material; Subsequently, raw material are inserted in the sintering oven being full of nitrogen and sinters, after terminating, namely obtain product; It is characterized in that, described catalyzer is iron powder; The sintering process of described sintering oven is: temperature is raised to top temperature 1300 ~ 1500 DEG C for 6 hours; Described vanadium oxide is at least one in Vanadium Pentoxide in FLAKES, vanadium tetraoxide, vanadous oxide.
2. the preparation method of VN alloy as claimed in claim 1, it is characterized in that, the ratio that described iron powder accounts for gross weight is: 0.3% ~ 1.5%.
3. the preparation method of VN alloy as claimed in claim 1, it is characterized in that, the ratio that described iron powder accounts for gross weight is 1.2%.
4. the preparation method of VN alloy as claimed in claim 1, is characterized in that, when the carrying out of described sintering oven sinters, under top temperature, is incubated 2 ~ 4 hours.
CN201510001232.3A 2015-01-05 2015-01-05 Method for preparing vanadium-nitrogen alloy Pending CN104531999A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510001232.3A CN104531999A (en) 2015-01-05 2015-01-05 Method for preparing vanadium-nitrogen alloy

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510001232.3A CN104531999A (en) 2015-01-05 2015-01-05 Method for preparing vanadium-nitrogen alloy

Publications (1)

Publication Number Publication Date
CN104531999A true CN104531999A (en) 2015-04-22

Family

ID=52847617

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510001232.3A Pending CN104531999A (en) 2015-01-05 2015-01-05 Method for preparing vanadium-nitrogen alloy

Country Status (1)

Country Link
CN (1) CN104531999A (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106276824A (en) * 2016-07-27 2017-01-04 河北钢铁股份有限公司承德分公司 A kind of method preparing high nitrogen vanadium nitride with coke
CN106315524A (en) * 2016-07-28 2017-01-11 河北钢铁股份有限公司承德分公司 Method for producing vanadium nitride through pushed slab kiln
CN106399786A (en) * 2016-11-25 2017-02-15 南通汉瑞新材料科技有限公司 Novel method for preparing vanadium-nitrogen alloy
CN106555053A (en) * 2015-09-24 2017-04-05 陕西五洲钒金属材料科技有限公司 A kind of vanadic anhydride ball making method
CN111101051A (en) * 2019-11-05 2020-05-05 河钢股份有限公司承德分公司 Method for improving nitrogen content in vanadium-nitrogen alloy production process

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1480548A (en) * 2003-03-13 2004-03-10 东北大学 Vanadium nitrogen microalloy additive and its preparing method
CN104004934A (en) * 2014-04-30 2014-08-27 四川展祥特种合金科技有限公司 Method for rapid preparation of vanadium-nitrogen alloy

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1480548A (en) * 2003-03-13 2004-03-10 东北大学 Vanadium nitrogen microalloy additive and its preparing method
CN104004934A (en) * 2014-04-30 2014-08-27 四川展祥特种合金科技有限公司 Method for rapid preparation of vanadium-nitrogen alloy

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106555053A (en) * 2015-09-24 2017-04-05 陕西五洲钒金属材料科技有限公司 A kind of vanadic anhydride ball making method
CN106276824A (en) * 2016-07-27 2017-01-04 河北钢铁股份有限公司承德分公司 A kind of method preparing high nitrogen vanadium nitride with coke
CN106315524A (en) * 2016-07-28 2017-01-11 河北钢铁股份有限公司承德分公司 Method for producing vanadium nitride through pushed slab kiln
CN106315524B (en) * 2016-07-28 2019-03-15 河北钢铁股份有限公司承德分公司 A kind of method of pushed bat kiln production vanadium nitride
CN106399786A (en) * 2016-11-25 2017-02-15 南通汉瑞新材料科技有限公司 Novel method for preparing vanadium-nitrogen alloy
CN111101051A (en) * 2019-11-05 2020-05-05 河钢股份有限公司承德分公司 Method for improving nitrogen content in vanadium-nitrogen alloy production process
CN111101051B (en) * 2019-11-05 2021-09-10 河钢股份有限公司承德分公司 Method for improving nitrogen content in vanadium-nitrogen alloy production process

Similar Documents

Publication Publication Date Title
CN104531999A (en) Method for preparing vanadium-nitrogen alloy
CN103708455B (en) The method preparing carbide
CN103305739B (en) A kind of high nitrogen VN alloy VN18 and production method thereof
CN102041422B (en) Silicon nitride ferrovanadium and production method thereof
AU2012243313C1 (en) Post-sinter conglutination and oxidation-preventative vanadium-nitrogen alloy preparation method
CN101586172A (en) Method for preparing metallized pellet and reduced iron powder
CN101289713B (en) Production process of vanadium-nitrogen alloy
CN102644015A (en) Production method for vanadium nitride ferroalloy
CN104259470B (en) A kind of low pine is than the production method of high fine powder rate 100 order reduced iron powders
CN105132674A (en) Ferrochrome preparation method
CN101302580B (en) Preparation of all-sefstromite concentrate pellet ore
CN104018056A (en) Preparation method of nitrided ferrovanadium with high quality and low cost
CN102173395B (en) Simple vanadium nitride production method
CN106319124A (en) Preparing method for ferrochrome silicon alloy
CN100507012C (en) Producing process of directly reducing iron
CN104526189A (en) Method for reducing ilmenite through microwave composite reducing agents and preparing electrode coatings
CN102936678A (en) Vanadium-nitrogen alloy production method
CN106381384A (en) Method for preparing ferrovanadium through vacuum reduction
CN103014345A (en) Production method of vanadium-nitrogen alloy
CN103663555B (en) A kind of Granular vanadium oxide and production method thereof
CN103937971B (en) The preparation method of iron ore hot pressing carbon-containing pelletizing and iron-smelting raw material
CN102534219A (en) Preparation method of vanadium nitride iron alloys for preventing bonding after alloy sintering
CN103303880A (en) Production process for preparing high-nitrogen vanadium nitride by using vacuum furnace method
CN103011098A (en) Production method for increasing content of nitrogen in vanadium-nitrogen alloy
CN107974608A (en) A kind of ferrovanadium nitride and preparation method thereof

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C02 Deemed withdrawal of patent application after publication (patent law 2001)
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20150422