CN101693975B - Method for increasing nitrogen content of vanadium-nitrogen alloy - Google Patents
Method for increasing nitrogen content of vanadium-nitrogen alloy Download PDFInfo
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Abstract
The invention discloses a method for increasing the nitrogen content of vanadium-nitrogen alloy, comprising the following steps of adding a nitridation accelerator into a mixture comprising vanadium oxide, a carburizing agent, catalyst and a bonding agent, making material blocks, and heating the material blocks for gasifying or decomposing the nitridation accelerator to generate gas and form crisscrossed micro holes or channels in the material blocks. The nitrogen content is greatly increased as nitrogen in the nitridation reaction enters the inside of the material blocks through the holes or channels to participate in the reaction to result in completion of the nitridation reaction. Compared with the prior art, the invention solves the problems of accelerating carburization and intensifying nitridation from the carburization and oxidation mechanisms of vanadium-nitrogen alloy through adding nitridation accelerators into materials, thereby greatly increasing the nitrogen content of the vanadium-nitrogen alloy and simultaneously reducing the general production cost and energy consumption of the vanadium-nitrogen alloy.
Description
Technical field
The present invention relates to contain the barium oxide technical field of smelting.Relate in particular to a kind of employing and in containing barium oxide, add the method that nitrogenize promotor is improved nitrogen content of vanadium-nitrogen alloy.
Background technology
At present, VN alloy produce for the oxide compound of vanadium with addition of reductive agent, and in all kinds of smelting furnaces, reduce calcining or smelt.The oxide compound of vanadium is generally Vanadium Pentoxide in FLAKES and vanadous oxide, and by mix compression moulding and drying after carburization agent after, carbonization or nitrogenize are produced under hot conditions.The disadvantage of this method is the nitrogen content instability of product VN alloy (perhaps vanadium nitride), and fluctuation is big, can not stablize and produce the nitrogen content high product.
The cardinal principle that existing VN alloy (vanadium nitride) production technology is followed is expressed as follows with reaction equation: (1) VO (Gu)+2C (Gu)=VC (Gu)+CO (gas) ↑
(2) VO (Gu)+C (Gu)+CO (gas)=VC (Gu)+CO
2(gas) ↑
(3) VC (Gu)+1/2N
2(gas)=V (CN) (Gu)
We call carburizing reagent to reaction (1) and (2) traditionally, and the former is called direct carburizing reagent, and the latter is called indirect carburizing reagent; Reaction (3) becomes nitrogenizing reaction.These two kinds of reactions all are to carry out in the solid material piece of consolidation.From the process of reaction, gaseous product CO, the CO of carburizing reagent
2The key that can in the time of in time successfully discharging can reaction be carried out smoothly; Equally, can the key that carry out smoothly of nitrogenizing reaction then be the gas-nitrogen (N that participates in reaction
2) can enter smoothly.And the limitation of existing production technology maximum is exactly not deal with problems from the reaction process of aforementioned analysis, just works hard from concentration of reactants (for example excessive carbon), temperature of reaction, material piece degree of packing aspect.
For example Chinese patent 200610033096.7, name is called " a kind of production method of alloy of vanadium nitride ", be to be mixed by vanadium compound powder and carbonaceous material to be placed in the preparation stove, lead to again that the ammonia nitrogen mixed gas reduces, carbonization and nitrogenizing reaction and prepare vanadium nitride alloy powder.Chinese patent 200510031680.4, name is called " ferrovanadium nitride alloy and preparation method thereof ", is to carry out carbonization, nitrogenize and sintering reaction, disposable acquisition ferrovanadium nitride alloy simultaneously behind the compound that utilizes vanadium, carbon, the iron powder mixing briquetting in metallurgical furnace.These two kinds of preparation methods are by the production of carrying out alloy of vanadium nitride after carrying out nitrogenizing reaction with addition of carburization agent.Therefore, exist the nitrogen content fluctuation range big equally, production capacity is low, cost height, the problem that scale output is little.
Summary of the invention
The objective of the invention is in order to remedy the deficiencies in the prior art, on the basis of existing technology, study from the process of nitrogenizing reaction, solve the discharge and the problem that enters that participates in reactant gases of generated reactive gas, and by in batching, strengthening the dynamic conditions of carbonization, nitrogenize with addition of nitrogenize promotor, promote carburizing reagent and nitrogenizing reaction, finally reach the nitrogen content that improves VN alloy, obtain the purpose of the nitrogenous stable and vanadium-nitrogen alloy product that nitrogen content is higher.
The present invention realizes its purpose by the following technical solutions.
The present invention is a kind of method that improves nitrogen content of vanadium-nitrogen alloy, its innovative point is to by containing in the mixture that barium oxide, carburization agent, catalyzer, binding agent form with addition of nitrogenize promotor and finish mix, to the heating of material piece, make the gasification of nitrogenize promotor or decompose to produce gas, in the material piece, form crisscross microcosmic hole or passage; By these holes or passage, the nitrogen in the nitrogenizing reaction enters into inner participation of material piece and reacts, and makes nitrogenizing reaction complete, and nitrogen content increases; Its preparation method comprises the steps:
1) will contain barium oxide to be processed into-the 100--200 purpose is Powdered;
2) adding nitrogenize promotor and carburization agent, catalyzer are done and are mixed and mix;
3) outer adding additives carries out wet mixing and mixes;
4) compound after the wet mixing is pressed into material piece and heating and dry;
5) dried material piece is calcined under nitrogen protection;
6) come out of the stove behind the material piece furnace cooling after the calcining.
Material proportion of the present invention is (by weight): nitrogenize promotor: barium oxide=0.5～1.0: 100; Carburization agent: barium oxide=26-30: 100, catalyzer: barium oxide=0.5～1.0: 100, binding agent: barium oxide=0.5-1.5: 100.
Nitrogenize promotor of the present invention is ammonium sulfate, monoammonium sulfate, volatile salt, bicarbonate of ammonia, ammonium nitrate, ammonium chloride, ammonium poly-vanadate, ammonium meta-vanadate; Heavy oil, light oil; One or more of iron protocarbonate (TST); Contain barium oxide and be one or more of vanadous oxide, vanadium tetraoxide, Vanadium Pentoxide in FLAKES, vanadium monoxide and ammonium meta-vanadate, ammonium poly-vanadate; With finish mix piece under 200 ℃ of-1000 ℃ of temperature dry 40 hours-50 hours; To expect piece between 1450 ℃ of-1600 ℃ of calcination temperature range, calcine 20 hours-40 hours that cool to the furnace then below 100 ℃ and come out of the stove, obtaining nitrogen content is the VN alloy the finished product of 14%-18%.
Beneficial effect of the present invention is, compared with prior art, by adding nitrogenize promotor in batching, improved and strengthened the dynamic conditions of carbonization, nitrogenize, solved with existing method and produced the low and problem of unstable of nitrogen-containing alloy nitrogen content; The nitrogenize promotor of being adopted has makes advantages such as simple, cheap; Preparation cost of the present invention and energy consumption are all very low, can realize that the mass-producing of the nitrogen-containing alloy of high nitrogen content is produced, and satisfy the needs of market to the high nitrogen content product.Its technical thought and concrete preparation method all have advance at home and abroad.
Embodiment
Below describe formation mechanism of the present invention in detail and its implementation is described in conjunction with the embodiments.
The present invention starts with from the mechanism that VN alloy forms, employing is with addition of the method for nitrogenize promotor, strengthen the micro kinetics condition of carbonization, nitrogenize, promoted the carrying out of carbonization and nitrogenizing reaction, can very convenient, stably produce the VN alloy of high nitrogen content.
The present invention for the discharge that solves gas in the reaction process with enter problem, imagination many crisscross microcosmic duct or holes of formation in the material piece at first before carbonization and nitrogenizing reaction begin.The formation of these microchannel or hole both can have been adopted machinery, also can allow the material piece self form.The present invention adopts material piece self to form.When material piece self forms, adopt and in batching, add a kind of material that is called nitrogenize promotor.This material (was no more than 500 ℃ usually) and will gasifies or decompose generation gas before carburizing reagent begins, will form crisscross microchannel in the material piece in the process that gas is discharged.Gas in the reaction process then can discharge from these microchannel or enter, and reaches the purpose that promotes reaction, finally improves the nitrogen content of product.And these passages continue up to the nitrogenizing reaction end, and cooling is closed after shrinking voluntarily.
The barium oxide that contains of the present invention is a vanadous oxide, one or more of vanadium tetraoxide, Vanadium Pentoxide in FLAKES, vanadium monoxide and ammonium meta-vanadate, ammonium poly-vanadate.
Nitrogenize promotor of the present invention is: ammonium sulfate or monoammonium sulfate, volatile salt or bicarbonate of ammonia, ammonium nitrate, ammonium chloride; Ammonium poly-vanadate (APV), ammonium meta-vanadate (AMV); Heavy oil, light oil; One or more of iron protocarbonate (TST).These promotor can directly bought on the market.The maximum characteristics of these products are exactly to be lower than gas that all can decompose generation under 500 ℃ of temperature or the gas that self gasifies and produce.The gas that produces will inevitably pass the material piece layer of consolidation and discharge, on the path of discharging, will stay a series of crisscross microscopic channels or hole, these passages or hole just become the access way or the hole of gas in the subsequent reactions process naturally, close after nitrogenizing reaction finishes to cool.From this description as can be seen, nitrogenize promotor is not to rely on itself nitrogen content to increase (also is like this even itself contains nitrogen) of nitrogen content, but after forming the microscopic channels or hole of microcosmic by it, strengthened the nitrogenizing reaction process, make a large amount of nitrogen enter into material piece inside, changed original pattern that diffuses into, thereby increased the nitrogen amount that participates in nitrogenizing reaction by passage or hole, generate more vanadium nitride, thereby increased the nitrogen content of product.Be example with the iron protocarbonate only, it at first decomposes generation CO in calcination process
2Gas produces ferric oxide simultaneously, and the former can produce microchannel or hole, and the latter can be used as catalyzer and iron is provided, so iron protocarbonate or above other composition as nitrogenize promotor are nitrogenize promotor the most efficiently.
Carburization agent of the present invention is graphite and carbon black.
Catalyzer of the present invention is: iron powder.
Binding agent of the present invention is: flour, Tapioca Starch, spent pulping liquor, syrup, polyvinyl alcohol etc.Require the intensity of hygrometric state and dry state good, easy to use, environmental friendliness.
Material proportion of the present invention is (by weight): nitrogenize promotor: barium oxide=0.5～1.0: 100; Carburization agent: barium oxide=26-30: 100, catalyzer: barium oxide=0.5～1.0: 100, binding agent: barium oxide=0.5-1.5: 100.
The present invention adopt will contain barium oxide earlier and be finely ground to-the 100--200 purpose is Powdered, by weight percentage, according to conventional ratio or rational proportion by containing barium oxide, carburization agent, catalyzer, binding agent composition mixture, and then with 5～10: 100 ratio is with addition of nitrogenize promotor, and carry out 25-30 minute dry blend wet mixing, obtain uniform compound.
Doing and mixing purpose is in order to make composition even, to avoid the part flaws such as blackspot to occur because of batch mixing is uneven; Dry blend is carried out 25-30 minute wet mixing, the wet mixed feed that obtains mixing again with addition of binding agent with after adding water.The purpose of wet mixing is to help the processability that material is even, improve material.
The pressure that wet mixed feed is applied 10MPa-20MPa is pressed into 50 millimeters * 50 millimeters * 30 millimeters wet feed piece with it; The wet feed piece is heated under 200 ℃ of-1000 ℃ of temperature and in 50 hours-100 hours, carry out drying, obtain the siccative piece.Can remove the free water content more than 90% in the wet feed piece like this, avoid in follow-up calcination process producing a large amount of water and calciner is brought adverse influence.The siccative piece is carried out high temperature cabonization and calcining, and calcining temperature is 1450 ℃-1600 ℃, calcination time 20 hours-40 hours.High calcining temperature helps the contraction of product, improves the apparent density of product.Material piece after the calcining cools to the furnace below 100 ℃ comes out of the stove, and finally obtains the vanadium-nitrogen alloy product that nitrogen content is 14%-18%.
The nitrogenizing reaction that carries out when preparing VN alloy under principle of the present invention is more thorough, has increased the nitrogen amount that participates in nitrogenizing reaction, has generated more vanadium nitride, has increased the nitrogen content of product, and the nitrogen content of the finished product is than higher.
During great advantage of the present invention also has been to reduce and has produced to the dependence of control accuracy, even control accuracy is low in producing, because the reinforcement reaction process of gas in microchannel or hole of nitrogenizing reaction, make nitrogenizing reaction more thorough, the nitrogen content that can guarantee the product produced equally is in higher level, improves the output of VN alloy.
Therefore, by the preparation method of nitrogen content of vanadium-nitrogen alloy of the present invention, greatly improved the scale production and the economic benefit of VN alloy.The preparation method that its productivity ratio does not add the VN alloy of nitrogenize promotor will improve 50%, and quality is good, and cost reduces greatly.
The present invention has adopted best component and ratio in following embodiment, under the principle that does not break away from inventive concept, all components of the present invention or material all can obtain good effect in force.
Embodiment 1
With the vanadium tetraoxide of content of vanadium 60% and the mixture 1000kg of vanadium pentoxide powder, after being finely ground to-100 orders, with addition of graphite, 5kg iron powder, 5kg polyvinyl alcohol, the 5kg iron protocarbonate of 300kg, do to mix 25 minutes to evenly, add an amount of water wet mixing 25 minutes to evenly; The pressure that compound after the wet mixing is applied 9MPa is pressed into 50 millimeters * 50 millimeters * 30 millimeters wet feed piece, and the wet feed piece heats under 200 ℃ of temperature and dry 50 hours, obtains the siccative piece; The siccative piece is carried out the constant-pressure and high-temperature carbonization and calcine in nitriding furnace, 1550 ℃ of calcining temperatures are come out of the stove below the calcination time 28 hours, agglomerating material piece furnace cooling to 100 ℃, have obtained nitrogen content and be 17.50% vanadium-nitrogen alloy product.
This embodiment is because of with addition of nitrogenize promotor, and the output of per 24 hours production VN alloy is 1500kg, then has only 1000kg with addition of the output of nitrogenize promotor.
Embodiment 2
After the mixture 1000kg of the vanadous oxide of content of vanadium 61% and vanadium tetraoxide powder is finely ground to-100 orders, carbon black, 6kg iron powder, 7kg flour, 6kg ammonium chloride with addition of 290kg, do to mix 25 minutes to evenly, add an amount of water wet mixing 25 minutes to evenly; The pressure that compound after the wet mixing is applied 9MPa is pressed into 50 millimeters * 50 millimeters * 30 millimeters wet feed piece, and the wet feed piece heats under 200 ℃ of temperature and dry 50 hours, obtains the siccative piece; The siccative piece is carried out the constant-pressure and high-temperature carbonization and calcine in nitriding furnace, 1550 ℃ of calcining temperatures are come out of the stove below the calcination time 28 hours, agglomerating material piece furnace cooling to 100 ℃, have obtained nitrogen content and be 16.80% vanadium-nitrogen alloy product.
This embodiment is because of with addition of nitrogenize promotor, and the output of per 24 hours production VN alloy is 1520kg, then has only 1000kg with addition of the output of nitrogenize promotor.
Embodiment 3
After the vanadium tetraoxide powder 1000kg of content of vanadium 62% is finely ground to-200 orders,, does and mix 25 minutes to evenly, add an amount of water wet mixing 25 minutes to evenly with addition of graphite, 7kg iron powder, 9kg polyvinyl alcohol, the 8kg ammonium sulfate of 285kg; The pressure that compound after the wet mixing is applied 9MPa is pressed into 50 millimeters * 50 millimeters * 30 millimeters wet feed piece, and the wet feed piece heats under 200 ℃ of temperature and dry 50 hours, obtains the siccative piece; The siccative piece is carried out the constant-pressure and high-temperature carbonization and calcine in nitriding furnace, 1550 ℃ of calcining temperatures are come out of the stove below the calcination time 28 hours, agglomerating material piece furnace cooling to 100 ℃, have obtained nitrogen content and be 18.00% vanadium-nitrogen alloy product.
This embodiment is because of with addition of nitrogenize promotor, and the output of per 24 hours production VN alloy is 1570kg, then has only 1000kg with addition of the output of nitrogenize promotor.
Embodiment 4
After the mixture 1000kg of the vanadous oxide of content of vanadium 63% and ammonium meta-vanadate powder is finely ground to-160 orders, carbon black, 9kg iron powder, 11kg Tapioca Starch, 9kg bicarbonate of ammonia with addition of 278kg, do to mix 25 minutes to evenly, add an amount of water wet mixing 25 minutes to evenly; The pressure that compound after the wet mixing is applied 9MPa is pressed into 50 millimeters * 50 millimeters * 30 millimeters wet feed piece, and the wet feed piece heats under 200 ℃ of temperature and dry 50 hours, obtains the siccative piece; The siccative piece is carried out the constant-pressure and high-temperature carbonization and calcine in nitriding furnace, 1600 ℃ of calcining temperatures are come out of the stove below the calcination time 24 hours, agglomerating material piece furnace cooling to 100 ℃, have obtained nitrogen content and be 16.00% vanadium-nitrogen alloy product.
This embodiment is because of with addition of nitrogenize promotor, and the output of per 24 hours production VN alloy is 1550kg, then has only 1000kg with addition of the output of nitrogenize promotor.
Embodiment 5
After the vanadous oxide powder 1000kg of content of vanadium 65% is finely ground to-160 orders,, does and mix 25 minutes to evenly, add an amount of water wet mixing 25 minutes to evenly with addition of graphite, 10kg iron powder, 15kg syrup, the 10kg heavy oil of 260kg; The pressure that compound after the wet mixing is applied 9MPa is pressed into 50 millimeters * 50 millimeters * 30 millimeters wet feed piece, and the wet feed piece heats under 300 ℃ of temperature and dry 45 hours, obtains the siccative piece; The siccative piece is carried out the constant-pressure and high-temperature carbonization and calcine in nitriding furnace, 1530 ℃ of calcining temperatures are come out of the stove below the calcination time 27 hours, agglomerating material piece furnace cooling to 100 ℃, have obtained nitrogen content and be 14.70% vanadium-nitrogen alloy product.
This embodiment is because of with addition of nitrogenize promotor, and the output of per 24 hours production VN alloy is 1550kg, then has only 1000kg with addition of the output of nitrogenize promotor.
The present invention starts with from high temperature cabonization, the nitridation mechanism of VN alloy, by in batching, adding nitrogenize promotor, solve accelerated carbonation, strengthened the difficult problem of nitrogenize, compare with existing method, significantly improved the nitrogen content of VN alloy, and can guarantee more than 14.0%.Simultaneously, the comprehensive production cost of VN alloy, energy consumption all have reduction significantly.
Nitrogen content of vanadium-nitrogen alloy promotor preparation of the present invention is simple, raw material is easy to get, reliable in quality; The present invention is applicable to that high temperature cabonization, nitriding produce the nitrogen-containing alloy of rare metal, to some nitrogen-containing alloys that is difficult to obtain with traditional nitriding method high nitrogen content, uses method of the present invention, can stablize, produce efficiently the product that obtains high vanadium nitrogen amount.
Claims (9)
1. method that improves nitrogen content of vanadium-nitrogen alloy, it is characterized in that to by containing in the mixture that barium oxide, carburization agent, catalyzer, binding agent form with addition of nitrogenize promotor and finish mix, to the heating of material piece, make the gasification of nitrogenize promotor or decompose to produce gas, in the material piece, form crisscross microcosmic hole or passage; By these holes or passage, the nitrogen in the nitrogenizing reaction enters into inner participation of material piece and reacts, and makes nitrogenizing reaction complete, and nitrogen content increases; Specifically comprise the steps:
1) will containing barium oxide, to be processed into-100～-200 purposes Powdered;
2) adding nitrogenize promotor and carburization agent, catalyzer are done and are mixed and mix;
3) outer adding additives carries out wet mixing and mixes;
4) compound after the wet mixing is pressed into material piece and heating and dry;
5) dried material piece is calcined under nitrogen protection;
6) come out of the stove behind the material piece furnace cooling after the calcining;
The calcining temperature of described material piece is 1450 ℃-1600 ℃, calcination time 20 hours-40 hours;
The material proportion that described material piece adopts is for by weight: nitrogenize promotor: barium oxide=0.5～1.0: 100; Carburization agent: barium oxide=26-30: 100, catalyzer: barium oxide=0.5～1.0: 100, binding agent: barium oxide=0.5-1.5: 100.
2. the method for raising nitrogen content of vanadium-nitrogen alloy according to claim 1 is characterized in that described nitrogenize promotor is ammonium sulfate, monoammonium sulfate, volatile salt, bicarbonate of ammonia, ammonium nitrate, ammonium chloride, ammonium poly-vanadate, ammonium meta-vanadate; Heavy oil, light oil; One or more of iron protocarbonate.
3. the method for raising nitrogen content of vanadium-nitrogen alloy according to claim 1 is characterized in that the described barium oxide that contains is one or more of vanadous oxide, vanadium tetraoxide, Vanadium Pentoxide in FLAKES.
4. the method for raising nitrogen content of vanadium-nitrogen alloy according to claim 3 is characterized in that the described barium oxide that contains is a vanadous oxide.
5. the method for raising nitrogen content of vanadium-nitrogen alloy according to claim 1 is characterized in that described carburization agent is one or both of graphite or carbon black.
6. the method for raising nitrogen content of vanadium-nitrogen alloy according to claim 1 is characterized in that described catalyzer is an iron powder.
7. the method for raising nitrogen content of vanadium-nitrogen alloy according to claim 1 is characterized in that described binding agent is one or more of flour, Tapioca Starch, spent pulping liquor, syrup, polyvinyl alcohol.
8. the method for raising nitrogen content of vanadium-nitrogen alloy according to claim 1 is characterized in that described material piece under 200 ℃ of-1000 ℃ of temperature dry 40 hours-50 hours.
9. the method for raising nitrogen content of vanadium-nitrogen alloy according to claim 1 is characterized in that described material piece cools to the furnace below 100 ℃ to come out of the stove, and obtains the VN alloy that nitrogen content is 14%-18%.
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| CN1587064A (en) * | 2004-08-05 | 2005-03-02 | 常州市茂盛特合金制品厂 | Process for producing vanadium nitrate |
| CN101003867A (en) * | 2006-01-20 | 2007-07-25 | 蔡惜辉 | Method for preparing alloy of vanadium nitride |
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