CN103846425A - Nitrogen-molybdenum alloy preparing method - Google Patents
Nitrogen-molybdenum alloy preparing method Download PDFInfo
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- CN103846425A CN103846425A CN201210508030.4A CN201210508030A CN103846425A CN 103846425 A CN103846425 A CN 103846425A CN 201210508030 A CN201210508030 A CN 201210508030A CN 103846425 A CN103846425 A CN 103846425A
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Abstract
The invention discloses a nitrogen-molybdenum alloy preparing method. The method includes feeding metal molybdenum powder into a reactor in a manner of spiral conveying, inputting ammonia gas in the opposite direction, rotating continuously, feeding and discharging material continuously, and obtaining the nitrogen-molybdenum alloy by decomposing through the ammonia gas and nitriding. The nitrogen-molybdenum alloy is powdered, with the nitrogen content ranging from 10 to 20%, and contains less than 0.5% of other elements, except for molybdenum element, , and the balance of molybdenum. The method ensures ease of obtaining raw materials, process is stable, and the method is adaptable to continuous production and large-scale industrial production.
Description
Technical field
The preparation method who the present invention relates to a kind of molybdenum nitrogen alloy, belongs to the field of new such as special alloy steel, Aero-Space, petrochemical industry, electronic apparatus.
Background technology
Molybdenum is a kind of rare refractory metal: molybdenum nitrogen alloy has the characteristics such as high-melting-point, high rigidity, good thermal stability and mechanically stable, can strengthen intensity, hardness, weldability and the toughness of alloy, also can strengthen its high temperature resistant and decay resistance.Molybdenum nitrogen alloy also has electronic structure and the good capacitive characteristics of similar noble metal and discharges and recharges behavior, also have catalysis characteristics, in hydrodesulfurization reaction, show the superperformance that is better than current commercial catalyst, demonstrate good activity, some performance even approaches or is better than traditional noble metal catalyst thereby is described as " accurate platinum catalyst " is the catalyst new material that a class is rich in hope, also be to smelt new material, electronic apparatus new material, be widely used in special alloy steel, Aero-Space, petrochemical industry, the fields such as electronic apparatus, molybdenum nitrogen alloy has significantly senior energy-conservation, environmental protection, the features such as safety, has promotional value.
Chinese patent (application): the method for preparing molybdenum nitride that 201110101655.4 analogy China disclose in the preparation method of molybdenum nitride is: ammoniacal liquor is as solvent, by ammonium molybdate and hexa in mass ratio 3.5:6 be mixed in ammoniacal liquor, after 60 ℃ of dry 24-26h, carry out roasting, 800 ℃ of temperature, 15h obtains Mo
2n.
Chinese patent (application): disclose in the preparation method that 02130058.5 Chen Hao chats about at molybdenum nitride and the application as Hydrobon catalyst thereof: by MoO
3under the nitrogen of proportioning certain purity and the mixed atmosphere of hydrogen, carry out multi-stage procedure temperature reaction, then cooling in inert atmosphere, passivation under certain oxygen concentration.
Chinese patent: 02113087.6 model is to disclose in the two rare selective hydrocatalyst molybdenum nitrides of peaceful long-chain normal and nitrogen molybdenum oxide and preparation and application: with MoO
3for raw material NH
3and H
2mist be nitridizing agent, adopt temperature programmed nitridation legal system standby.
The shortcoming of above-mentioned three patents is that employing molybdenum trioxide or ammonium molybdate are raw material, and production process has the three wastes and production security problem.Adopting nitridizing agent is nitrogen or ammonia and hydrogen gas mixture, dosing apparatus is cumbersome, also there is safety issue, heating all adopts calcination procedure to heat up, and gas waste is large, and nitrogenize efficiency is low, solid material and gas all can not carry out reactor continuously, single stove gap produces, and the thermal efficiency is low, and production efficiency is relative also lower.
In sum, in existing preparation method, none can the technology of production nitrogen content between 10-20%, is not also suitable for technology extensive and that produce continuously molybdenum nitrogen alloy.
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Summary of the invention
The present invention needs that technical solution problem is to provide that a kind of raw material is easy to get, stable technical process, produce continuously, is applicable to the preparation method of a kind of molybdenum nitrogen alloy that industrialization in enormous quantities produces.
Technical problem to be solved by this invention realizes by the following technical solutions:
A preparation method for molybdenum nitrogen alloy, is characterized in that: take metal molybdenum powder as raw material, ammonia is reaction medium, and its preparation process is as follows:
Step 1: the control of reactor
Open reactor, and to the upper temperature-raising region temperature raising to 600 ℃ of reactor, high-temperature region is warmed up to 900 ℃;
Step 2: will drop in conveying worm material-storing box with the metal molybdenum powder of input 100KG per hour, and send in reactor by the mode of screw propulsion, pass through ammonia to opposite direction simultaneously;
Step 3: the passing into of ammonia
Anhydrous ammonia tank valve is opened, liquefied ammonia enters in ammonia vaporizer, start warm water valve, ammonia enters successively autocontrol valve, control plate flowmeter, ammonia autoalarm amputator and passes in reactor in the other direction in continual mode, and control between the air pressure 0.10 ~ 0.25Mpa in reactor, open air bleeding valve simultaneously, and start incinerator;
Step 4: nitridation reaction
In reactor, meet pyrolytic and become hydrogen and ammonia when the ammonia in step 3 enters, hydrogen volume is larger, can be full of rapidly whole reactor, ammonia is rapid and metal molybdenum powder generation nitridation reaction, and generating molybdenum nitrogen alloy, unnecessary hydrogen burns in reactor exhaust outlet enters hydrogen incinerator;
Step 5: need stop 6h to the whole process of reactor tail end by rotary moving the molybdenum nitrogen alloy obtaining after nitridation reaction, the absolute pressure of ammonia is 0.15Mpa, then carry out after 100 ℃ of < cool, discharge reactor through sealed discharging device and enter finished product box, finally obtain pulverous molybdenum nitrogen alloy.
Described raw material choose metal molybdenum powder is 80 ~ 120 orders, Mo content >=99.50 ~ 99.90%, Si:0.005%, C:0.03%, P:0.005%, Fe:0.10%, O:0.15%.
The course of reaction of described whole step is all to complete in reactor.
Described step 2 and step 3 are all to adopt incessantly to feed intake, pass into and emission gases.
Described reactor is stainless steel reacting in rotary kiln device.
The invention has the beneficial effects as follows:
1. the nitrogen content in the molybdenum nitrogen alloy of this explained hereafter can reach between 10-20%, far away higher than the nitrogen content of existing other production technology;
2. the molybdenum nitrogen alloy of this explained hereafter, except molybdenum, nitrogen, the every other composition total content of adding up is less than 0.5%, other impurity very low as: Si<0.004%, C<0.01%, P<0.005%, Fe < 0.10, O < 0.25;
3. this technique is using molybdenum powder as raw material, ammonia completes whole production process as medium in stainless steel sealing reacting in rotary kiln device, this preparation method's cost is low, low, the simple process, safe that consumes energy, and automaticity is high, high, good in economic efficiency without the three wastes (environmental protection industry), yield;
4. this process using consecutive production method of solid material and gaseous feed of being back to back, the thermal efficiency is high, process stabilizing, constant product quality;
5. the product of this technique is Powdered, can multiple use, also can be made into core-spun yarn, and can also make bulk, also can use by powder.
The specific embodiment
For technological means, creation characteristic that the present invention is realized, reach object and effect is easy to understand, below in conjunction with specific embodiment, further set forth the present invention.
A preparation method for molybdenum nitrogen alloy, take metal molybdenum powder as raw material, ammonia is reaction medium, its preparation process is as follows:
1. the control of reactor
Open reactor, and to the upper temperature-raising region temperature raising to 600 ℃ of reactor, high-temperature region is warmed up to 900 ℃;
2. will drop in conveying worm material-storing box with the metal molybdenum powder of input 100KG per hour, and send in reactor by the mode of screw propulsion, pass through ammonia to opposite direction simultaneously;
3. passing into of ammonia
Anhydrous ammonia tank valve is opened, liquefied ammonia enters in ammonia vaporizer, start warm water valve, ammonia enters successively autocontrol valve, control plate flowmeter, ammonia autoalarm amputator and passes in reactor in the other direction in continual mode, and control between the air pressure 0.10 ~ 0.25Mpa in reactor, open air bleeding valve simultaneously, and start incinerator;
4. nitridation reaction
Ammonia in 3. enters meets pyrolytic in reactor and becomes hydrogen and ammonia, hydrogen volume is larger, can be full of rapidly whole reactor, ammonia is rapid and metal molybdenum powder generation nitridation reaction, and generating molybdenum nitrogen alloy, unnecessary hydrogen burns in reactor exhaust outlet enters hydrogen incinerator;
5. need stop 6h by rotary moving the molybdenum nitrogen alloy obtaining after nitridation reaction to the whole process of reactor tail end, the absolute pressure of ammonia is 0.15Mpa, then carry out after 100 ℃ of < cool, discharge reactor through sealed discharging device and enter finished product box, finally obtain pulverous molybdenum nitrogen alloy, wherein nitrogen content is between 10 ~ 15%, except molybdenum element, other composition constituent contents are less than 0.5%, and remaining is molybdenum element content entirely.
Products obtained therefrom is by analysis: wherein constituent content is as follows to obtain molybdenum nitrogen alloy:
| Element | Mn | N | Si | C | P | Fe | O |
| Content (%) | 85.14 | 14.61 | 0.004 | 0.01 | 0.003 | 0.08 | 0.10 |
The above-mentioned metal molybdenum powder of selecting is 80 ~ 120 orders, Mo content >=99.50 ~ 99.90%, Si:0.005%, C:0.03%, P:0.005%, Fe:0.10%, O:0.15%.
The course of reaction of whole step is all to complete in reactor above.
3. 2. step be all to adopt incessantly to feed intake, pass into and emission gases with step.
Reactor is stainless steel sealing reacting in rotary kiln device.
More than show and described basic principle of the present invention and principal character and advantage of the present invention.The technical staff of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and description, describes just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (5)
1. a preparation method for molybdenum nitrogen alloy, is characterized in that: take metal molybdenum powder as raw material, ammonia is reaction medium, and its preparation process is as follows:
The control of a, reactor
Open reactor, and to the upper temperature-raising region temperature raising to 600 ℃ of reactor, high-temperature region is warmed up to 900 ℃;
B, will drop in conveying worm material-storing box with the metal molybdenum powder of input per hour 100KG, and send in reactor by the mode of screw propulsion, pass through ammonia to opposite direction simultaneously;
Passing into of c, ammonia
Anhydrous ammonia tank valve is opened, liquefied ammonia enters in ammonia vaporizer, start warm water valve, ammonia enters successively autocontrol valve, control plate flowmeter, ammonia autoalarm amputator and passes in reactor in the other direction in continual mode, and control between the air pressure 0.10 ~ 0.25Mpa in reactor, open air bleeding valve simultaneously, and start incinerator;
D, nitridation reaction
In reactor, meet pyrolytic and become hydrogen and ammonia when the ammonia in step c enters, hydrogen volume is larger, can be full of rapidly whole reactor, ammonia is rapid and metal molybdenum powder generation nitridation reaction, and generating molybdenum nitrogen alloy, unnecessary hydrogen burns in reactor exhaust outlet enters hydrogen incinerator;
E, need stop 6h by rotary moving the molybdenum nitrogen alloy obtaining after nitridation reaction to the whole process of reactor tail end, the absolute pressure of ammonia is 0.15Mpa, then carry out after 100 ℃ of < cool, discharge reactor through sealed discharging device and enter finished product box, finally obtain pulverous molybdenum nitrogen alloy.
2. a kind of preparation method of molybdenum nitrogen alloy according to claim 1, is characterized in that: described raw material choose metal molybdenum powder is 80 ~ 120 orders, Mo content >=99.50 ~ 99.90%, Si:0.005%, C:0.03%, P:0.005%, Fe:0.10%, O:0.15%.
3. a kind of preparation method of molybdenum nitrogen alloy according to claim 1, is characterized in that: the course of reaction of described whole step is all to complete in reactor.
4. a kind of preparation method of molybdenum nitrogen alloy according to claim 1, is characterized in that: described step b and step c adopt incessantly to feed intake, pass into and emission gases.
5. a kind of preparation method of molybdenum nitrogen alloy according to claim 1, is characterized in that: described reactor is stainless steel sealing reacting in rotary kiln device.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1401580A (en) * | 2002-08-19 | 2003-03-12 | 中国科学院山西煤炭化学研究所 | Process for preparing molybdenum nitride and use thereof as hydrogenation and desulfurizing catalyst |
| CN1887421A (en) * | 2005-06-29 | 2007-01-03 | 中国科学院金属研究所 | Process and apparatus for preparing metal nitride catalyst material |
| CN1966150A (en) * | 2005-11-14 | 2007-05-23 | 中国科学院金属研究所 | Apparatus and method for preparing metal nitride catalytic material |
| CN101082088A (en) * | 2006-11-06 | 2007-12-05 | 王国宁 | Production technique for preparing high-purity high-nitrogen nitrogenization manganese metal |
| CN101172586A (en) * | 2007-09-30 | 2008-05-07 | 冯良荣 | Method for producing manganese nitride |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1560617A1 (en) * | 1988-03-01 | 1990-04-30 | Предприятие П/Я А-1278 | Method of nitriding molybdenum inserts of press-moulds |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1401580A (en) * | 2002-08-19 | 2003-03-12 | 中国科学院山西煤炭化学研究所 | Process for preparing molybdenum nitride and use thereof as hydrogenation and desulfurizing catalyst |
| CN1887421A (en) * | 2005-06-29 | 2007-01-03 | 中国科学院金属研究所 | Process and apparatus for preparing metal nitride catalyst material |
| CN1966150A (en) * | 2005-11-14 | 2007-05-23 | 中国科学院金属研究所 | Apparatus and method for preparing metal nitride catalytic material |
| CN101082088A (en) * | 2006-11-06 | 2007-12-05 | 王国宁 | Production technique for preparing high-purity high-nitrogen nitrogenization manganese metal |
| CN101172586A (en) * | 2007-09-30 | 2008-05-07 | 冯良荣 | Method for producing manganese nitride |
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Granted publication date: 20160217 Termination date: 20171203 |