CN101082088A - Production technique for preparing high-purity high-nitrogen nitrogenization manganese metal - Google Patents
Production technique for preparing high-purity high-nitrogen nitrogenization manganese metal Download PDFInfo
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- CN101082088A CN101082088A CN 200610032525 CN200610032525A CN101082088A CN 101082088 A CN101082088 A CN 101082088A CN 200610032525 CN200610032525 CN 200610032525 CN 200610032525 A CN200610032525 A CN 200610032525A CN 101082088 A CN101082088 A CN 101082088A
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Abstract
The present invention is technological process of producing Mn-N alloy with high purity and high N content. The technological process includes the following steps: crushing electrolytic metal Mn into Mn powder of 60 mesh, setting the Mn powder into a high vacuum resistive smelting furnace, vacuumizing and filling 99.99 % purity N2 to reach 0.2-0.25 MPa, heating with two voltage adjustable transformers for sintering and nitriding at 7 00-900 deg.c, and cooling gradually. The process is superior and can obtain Mn-N alloy with N content as high as 8-10 % and very low impurity content.
Description
Technical field
The present invention is the new production process technology of a kind of production high nitrogen high-purity manganese nitrogen zoarium (nitrogenized manganese).Manganese nitrogen zoarium is mainly used in steel alloy, the stainless steel smelting production of multicomponent, is the indispensable alloying constituents in field such as automobile, shipbuilding, aircraft industry, nuclear industry material, and nitrogen is to belong to the element that enlarges the austenitic area.In recent years, especially manganese and nitrogen substitute the nickel The Application of Technology in the stainless steel, and high nitrogen steel is considered to one of direction of Future Development high quality metallurgical technology, and product of the present invention------manganese nitrogen zoarium, one of important materials of this field application just.
Background technology
The fit manufacturer of manganese nitrogen is few at present, and its production method is also just with manganese metal or the logical nitrogen of ferromanganese heating.The product nitrogen content that obtains of method is low thus, and impurity element height, and yielding poorly is produced waywardly, and quality product can not be stablized.The present Jilin Iron Alloy Plant of reference (lucky Q/JT.H42-27-95 standard, their product index are N:4--6%, Mn 〉=90%, and C＜0.05%, P＜0.05% can't be referred to as the high-purity nitrogenized manganese product of high nitrogen.In addition, domestic also have some to utilize the ammonia decomposition method to carry out the preparation of nitrogenized manganese, but this method nitrogen content can only reach 6.8%--6.9%, and this method is difficult for industrialization, dangerous property and influential to environment, and the more existing processing method for preparing high nitrogen manganese nitrogen zoarium also only just is confined to the laboratory at present, inreal realization scale production.
Summary of the invention
The purpose of this invention is to provide a kind of is raw material with the high-purity electrolytic metal manganese powder more than 60 orders, and warm nitridation sintered method is produced the production technique of high nitrogen manganese nitrogen zoarium in the employing in vacuum resistance furnace.
Process technology scheme feature of the present invention is as follows:
1. high-purity electrolytic metal Mn (Mn content 〉=99.7%) is broken into the above manganese powder of 60 orders, is positioned on the rail mounted material dolly, and the material dolly is pushed in the vacuum oven, and the airtight vacuum smelting furnace.Discover that the size range of raw material that this technology adopts helps the combination of nitrogen manganese most;
2. use the vacuum pump unit of two class large power high vacuum,, the invention reside in and regulate the appropriate vacuum degree index, be beneficial to provide nitrogen manganese sintering best atmosphere with vacuum tightness in certain pumping speed control vacuum oven.This production technique optimal vacuum pressure is 10Pa;
3. utilize high pure nitrogen source (N
2〉=99.99%) in vacuum smelting furnace, fills nitrogen with certain speed, take into account by-pass valve control regulation and control fill rate by flow, and finally to control furnace atmosphere pressure be a optimum value between the 0.15MPa--0.25MPa, and this technology is to have determined one and helps nitrogen manganese agglomerating gaseous tension scope most;
4. this production technique uses 2 800KVA ULTCs to send electricity to the carbon-point rod of vacuum smelting furnace, and electrode voltage can many grades of pressure regulation, so that accurately control the temperature required in the stove and the speed of temperature rise.Technology controlling and process optimum parameter of the present invention is a certain value between 700--900 ℃, and with certain temperature rise speed, will help nitrogen most and permeate in manganese, reaches the target of high nitrogen;
5. under optimum temps and pressure, be incubated, pressurize.In the present invention, found a suitable time value to keep state of the art, promptly be incubated 5---8 hour under suitable temperature and pressure, so more helped the infiltration and the homogeneous phaseization of nitrogen, this is the key that reaches high nitrogen content;
6. this production technique adopts best cooling chart that vacuum oven is carried out slowly grand temperature drop to press, under convenient pressure, and when temperature reaches between 200--250 ℃ a certain value, unlatching vacuum oven, extract trolley.For the blow-on temperature controlling is to guarantee that nitrogen manganese in conjunction with the stabilization of phase and the key that prevents the manganese burning, is to guarantee to obtain the particularly important technical index of high purity product of high nitrogen.
The present invention has following characteristics and advantage
At first, adopt that nitrogen content can reach 8%--10% in the manganese nitrogen zoarium of this explained hereafter, be higher than the nitrogen content that existing other production technique draws product far away, production technique for other has the superiority that can't compare, and this product is impure very low, S＜0.005%, C＜0.04%, P＜0.005%,, be much better than other like product;
Secondly, production technique of the present invention has realized industrial sector production, adopts same transformer bank to be powered at two vacuum ovens in turn, can realize continual production, and the output of every day can reach the 6--8 ton, is that other production technique is incomparable;
The 3rd, temperature was filled nitrogen and is carried out sintering during the present invention adopted, and energy consumption is low, and technology controlling and process is accurate, and products production efficient is high and stable, and environmentally safe does not have other technology such as environmental protection that brings with the ammonia decomposition technique and security problems.
Description of drawings
Fig. 1 is the process flow sheet that is used to prepare high-purity high-nitrogen nitrogenization manganese metal of the present invention.
Embodiment
With electrolytic manganese (C=0.08% P=0.005%) is crushed to more than 60 orders for Mn=99.7%, S=0.03%, the convey materials dolly of packing into, every chassis is put 1.5 tons, puts 4 cars and amounts to 6 tons, and 4 dollies are pushed vacuum smelting furnace and airtight;
2. vacuum oven is vacuumized, final vacuum tightness is 12Pa; Fill N
2(purity 〉=99.99%) to stove, final furnace pressure is 0.21MPa;
3. starting transformer, vacuum oven electrode, vacuum oven cooling water circulation system are carried out the pressure regulation temperature adjustment, and temperature is slow to be risen between 806--835 ℃, and insulation is handled;
4. when slow cooling temperature is reduced to 246 ℃, open fire door, take out material;
5. material is cooled to room temperature, is broken for 10mm * 10mm bulk, metering, packing warehouse-in, and this time production process draws product through by analysis, obtains manganese nitrogen nitrogen zoarium, wherein following (the unit: %) of constituent content
| Element | Mn | ?N | ?S | ?C | ?P |
| Content (%) | 87.77 | ?8.73 | ?0.004 | ?0.01 | ?0.003 |
Claims (1)
1. the present invention relates to a kind of production technique for preparing high-purity high-nitrogen nitrogenization manganese metal, it is that the electrolytic metal manganese powder is placed in the vacuum smelting furnace, vacuumizes, fills nitrogen, middle temperature nitriding agglomerating process, it is characterized in that:
A. be that raw material is positioned in the airtight vacuum smelting furnace with the high-purity electrolytic metal Mn more than 60 orders (Mn content 〉=99.7%) powder;
B. technology of the present invention is with vacuum tightness in certain pumping speed control vacuum oven, and it is about 10Pa that the present invention regulates the appropriate vacuum degree index, is beneficial to provide nitrogen manganese sintering best atmosphere;
C. utilize high pure nitrogen source (N
2〉=99.99%) fill nitrogen with certain speed in vacuum smelting furnace, this technology is to have determined one, and to help nitrogen manganese agglomerating gaseous tension scope most be 0.20Mpa----0.25MPa;
D. the best nitriding sintering temperature of this controlling of production process parameter is a certain value between the 700--900 ℃ of sintering;
E. under optimum temps and pressure, be incubated, the control of time of pressurize, its time scope is 5-8 hour;
F. vacuum oven being carried out decrease temperature and pressure control is to guarantee that nitrogen manganese in conjunction with the stabilization of phase and the key that prevents the manganese burning, is to guarantee to obtain the particularly important technical index of high purity product of high nitrogen, and the best blow-on temperature of this technology is 200----250 ℃.
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| CNB2006100325259A CN100497686C (en) | 2006-11-06 | 2006-11-06 | Production technique for preparing high-purity high-nitrogen nitrogenized manganese metal |
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| CNB2006100325259A CN100497686C (en) | 2006-11-06 | 2006-11-06 | Production technique for preparing high-purity high-nitrogen nitrogenized manganese metal |
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| CN101082088A true CN101082088A (en) | 2007-12-05 |
| CN100497686C CN100497686C (en) | 2009-06-10 |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102910597A (en) * | 2012-10-31 | 2013-02-06 | 中信锦州金属股份有限公司 | Method for increasing nitriding quantity of manganese nitride in nitride smelting process |
| CN103803512A (en) * | 2014-02-28 | 2014-05-21 | 大连理工大学 | Tetramanganese nitride, preparation method of tetramanganese nitride, absorbent containing tetramanganese nitride and preparation method of absorbent |
| CN103846425A (en) * | 2012-12-03 | 2014-06-11 | 安徽港铭新材料科技有限公司 | Nitrogen-molybdenum alloy preparing method |
| CN103849829A (en) * | 2012-12-03 | 2014-06-11 | 安徽港铭新材料科技有限公司 | Preparation method for manganese-nitrogen alloy |
| CN107010610A (en) * | 2017-06-13 | 2017-08-04 | 王兆兵 | A kind of energy-efficient high purity silicon nitride manganese production system |
| CN107140610A (en) * | 2017-06-13 | 2017-09-08 | 王兆兵 | A kind of energy-efficient high purity silicon nitride manganese production method |
| CN110272029A (en) * | 2019-08-02 | 2019-09-24 | 湘西自治州丰达合金科技有限公司 | A kind of preparation method of high purity silicon nitride manganese |
| CN110468315A (en) * | 2019-08-30 | 2019-11-19 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of preparation method of richness nitrogen manganese vanadium-based materials |
| CN110482502A (en) * | 2019-10-05 | 2019-11-22 | 王兆兵 | A kind of energy-efficient manganese nitride production process |
| CN113840673A (en) * | 2019-02-26 | 2021-12-24 | 索尼奥环球控股有限责任公司 | High-nitrogen steel powder and manufacturing method thereof |
| CN115125392A (en) * | 2022-08-18 | 2022-09-30 | 湘西自治州丰达合金科技有限公司 | Manganese nitride ball production process |
| CN115259110A (en) * | 2022-08-10 | 2022-11-01 | 湘西自治州丰达合金科技有限公司 | Process for controlling nitrogen content in manganese nitride |
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2006
- 2006-11-06 CN CNB2006100325259A patent/CN100497686C/en not_active Expired - Fee Related
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102910597A (en) * | 2012-10-31 | 2013-02-06 | 中信锦州金属股份有限公司 | Method for increasing nitriding quantity of manganese nitride in nitride smelting process |
| CN103846425A (en) * | 2012-12-03 | 2014-06-11 | 安徽港铭新材料科技有限公司 | Nitrogen-molybdenum alloy preparing method |
| CN103849829A (en) * | 2012-12-03 | 2014-06-11 | 安徽港铭新材料科技有限公司 | Preparation method for manganese-nitrogen alloy |
| CN103846425B (en) * | 2012-12-03 | 2016-02-17 | 安徽港铭新材料科技有限公司 | A kind of preparation method of molybdenum nitrogen alloy |
| CN103849829B (en) * | 2012-12-03 | 2016-12-21 | 安徽港铭新材料科技有限公司 | A kind of preparation method of manganese nitrogen alloy |
| CN103803512A (en) * | 2014-02-28 | 2014-05-21 | 大连理工大学 | Tetramanganese nitride, preparation method of tetramanganese nitride, absorbent containing tetramanganese nitride and preparation method of absorbent |
| CN103803512B (en) * | 2014-02-28 | 2016-08-31 | 大连理工大学 | A kind of nitridation four manganese and preparation method thereof and the absorbent containing this kind of nitridation four manganese and preparation method thereof |
| CN107140610A (en) * | 2017-06-13 | 2017-09-08 | 王兆兵 | A kind of energy-efficient high purity silicon nitride manganese production method |
| CN107010610A (en) * | 2017-06-13 | 2017-08-04 | 王兆兵 | A kind of energy-efficient high purity silicon nitride manganese production system |
| CN107010610B (en) * | 2017-06-13 | 2023-09-19 | 王兆兵 | High-efficiency energy-saving high-purity manganese nitride production system |
| CN113840673A (en) * | 2019-02-26 | 2021-12-24 | 索尼奥环球控股有限责任公司 | High-nitrogen steel powder and manufacturing method thereof |
| CN110272029A (en) * | 2019-08-02 | 2019-09-24 | 湘西自治州丰达合金科技有限公司 | A kind of preparation method of high purity silicon nitride manganese |
| CN110272029B (en) * | 2019-08-02 | 2023-04-11 | 湘西自治州丰达合金科技有限公司 | Preparation method of high-purity manganese nitride |
| CN110468315A (en) * | 2019-08-30 | 2019-11-19 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of preparation method of richness nitrogen manganese vanadium-based materials |
| CN110468315B (en) * | 2019-08-30 | 2021-06-08 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method of nitrogen-rich manganese vanadium-based material |
| CN110482502A (en) * | 2019-10-05 | 2019-11-22 | 王兆兵 | A kind of energy-efficient manganese nitride production process |
| CN115259110A (en) * | 2022-08-10 | 2022-11-01 | 湘西自治州丰达合金科技有限公司 | Process for controlling nitrogen content in manganese nitride |
| CN115125392A (en) * | 2022-08-18 | 2022-09-30 | 湘西自治州丰达合金科技有限公司 | Manganese nitride ball production process |
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| CN100497686C (en) | 2009-06-10 |
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Assignee: Hunan Sanxing Manganese Industry Co., Ltd. Assignor: Wang Guoning Contract fulfillment period: 2009.6.30 to 2015.6.30 Contract record no.: 2009430000097 Denomination of invention: Production technique for preparing high-purity high-nitrogen nitrogenization manganese metal Granted publication date: 20090610 License type: Exclusive license Record date: 20091019 |
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Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2009.6.30 TO 2015.6.30; CHANGE OF CONTRACT Name of requester: HUNAN SANXIN MANGANESE INDUSTRY SCIENCE AND TECHNO Effective date: 20091019 |
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