CN110482502B - Efficient and energy-saving manganese nitride production process - Google Patents
Efficient and energy-saving manganese nitride production process Download PDFInfo
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- CN110482502B CN110482502B CN201910946411.2A CN201910946411A CN110482502B CN 110482502 B CN110482502 B CN 110482502B CN 201910946411 A CN201910946411 A CN 201910946411A CN 110482502 B CN110482502 B CN 110482502B
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Abstract
The invention provides a high-efficiency energy-saving manganese nitride production process, which directly melts a manganese metal raw material into liquid, is atomized for the first time to be nitrided, is condensed into high-temperature powder and then is nitrided for the second time, has short production process, and can obtain manganese nitride powder by electrolyzing manganese metal sheets in one step. The manganese powder preparation and the nitriding are combined into a whole, the production is easy to realize automatic control, the production efficiency is high, the environmental pollution is small, the comprehensive production cost is low, and the power consumption can be controlled below 380 ℃ per ton of products.
Description
Technical Field
The invention relates to the field of additive production in ferrous metallurgy, in particular to a production technology of manganese nitride.
Background
The existing manganese nitride large-scale production is carried out in a large-scale vacuum nitriding furnace, is intermittent production, generally produces one batch in 24 hours, each batch is 4-10 tons, and the quality is stable and controllable, but has the following defects.
(1) The production energy consumption is high: the power consumption of each ton of the product is 450 degrees (the energy consumption for preparing the metal manganese powder is not contained), wherein the power consumption of the electric heating vacuum furnace is 370 degrees/ton of the product, and the power consumption of the vacuum furnace and the nitrogen preparation is 80 degrees/ton of the product.
(2) The total production process is long, and the comprehensive production cost is high: according to the manganese nitride powder with the largest market demand as an example, the production links have the following intermediate products: electrolytic manganese metal sheet (manganese metal block) → manganese metal powder → manganese forged and rolled ball → manganese nitride powder, at least crushing, mixing, forging, nitriding, crushing 5 processes, the overall cost is high. If the metal manganese powder is directly used for nitriding, the metal manganese powder is easy to sinter into blocks and needs to be crushed again, and the nitriding effect is poor and the nitrogen content is low after the metal manganese powder is sintered into blocks. Patent 2013106268813 directly removes fluidization nitridation with metal manganese powder, and metal manganese powder and nitrogen gas all need preheat earlier respectively, and system technological parameter is difficult to control, and the implementation degree of difficulty is big, and manufacturing cost is high.
(3) The environmental pollution is large: no matter manganese nitride powder or manganese nitride balls (pillows), metal manganese sheets (blocks) are required to be made into the metal manganese powder, the existing powder preparation method mainly adopts high-pressure roller milling or ball milling, the noise is high, in addition, vibration screening equipment is added, the raised dust is also large, although a dust collecting device is arranged, the system is not easy to seal, the leaked dust amount is still large, the harm to operators in the existing place is large, and the pollution to the surrounding environment is also large.
(4) The product quality needs to be continuously improved, the impurity content is high, the manganese-containing oxide is more, even if the electrolytic manganese metal sheet with high purity is used, the oxygen element content is 2% -3% through product detection, mainly because the manganese has active chemical property, the electrolytic manganese metal sheet can be oxidized and changed into black gray after being stored for a period of time though being passivated, after being crushed into manganese powder, the oxygen element content is 0.5% -1%, and after the links of adding water glass for mixing, forging and forming balls and drying, the manganese oxide is newly formed, so that the oxygen element content is up to 2.5% -3%. The technical proposal also proposes that the furnace is flushed with hydrogen-containing reducing gas such as ammonia pyrolysis gas, and the manganese oxide generated by reduction can only reduce a small part and has high production cost.
Disclosure of Invention
Aiming at the defects of the technology, the invention provides an efficient and energy-saving manganese nitride production process, which directly melts a manganese metal raw material (electrolytic manganese metal sheet or manganese metal block) into a liquid state, and is subjected to atomization and primary nitridation, and then is condensed into high-temperature powder and then is subjected to secondary nitridation, so that a large batch of high-quality manganese nitride products are obtained.
The specific technical scheme of the invention is as follows: the production process of manganese nitride is characterized by comprising the following steps.
Firstly, melting metal manganese: putting metal manganese into an electromagnetic induction smelting furnace, controlling the smelting temperature to 1350-1600 ℃ to obtain molten manganese liquid, and refining the molten manganese liquid to remove the upper-layer manganese oxide scum.
Secondly, primary atomization nitridation: introducing pure nitrogen into an atomizer, sucking molten manganese liquid into the atomizer, atomizing into small liquid drops in an atomizing chamber, introducing pure nitrogen into a Venturi powder sprayer, sucking the ultrafine metal manganese powder into the Venturi powder sprayer, then spraying into the atomizing chamber, colliding and adsorbing with the atomized manganese liquid drops, and condensing into powder; the recycling of the excessively fine metal manganese powder is realized, the manganese liquid is accelerated to be condensed, meanwhile, the cooling is enhanced in the atomizing chamber by using a cooling coil and a water cooling jacket, the nitrogen pressure of the atomizer is controlled to be 0.8-4 MPa, and the particle size of the powder is controlled to be 300-500 um; controlling the nitrogen pressure of the atomizing chamber to be 0.01 MPa-0.1 MPa and the temperature in the atomizing chamber to be 750-950 ℃.
Thirdly, secondary nitridation: depositing the hot manganese metal powder to the bottom of the atomizing chamber, introducing pure nitrogen from the bottom of the atomizing chamber, performing secondary boiling nitridation on the manganese metal powder, and controlling the nitridation temperature to be 750-950 ℃.
Fourthly, cooling and packaging: after secondary nitridation, the material is cooled to normal temperature by a cooler, the material discharged from a discharge outlet of the cooler is a manganese nitride powder product, powder-containing gas at an exhaust port of the cooler enters a primary separator, and fine powder discharged from a discharge outlet of the primary separator is also used as the manganese nitride powder product.
Further, the powder-containing gas discharged from the exhaust port of the primary separator enters the secondary separator and then enters the dust remover, the fine powder discharged from the secondary separator and the discharge port of the dust remover enters the atomizing chamber through the venturi powder sprayer for recycling, the tail gas at the outlet of the dust remover enters the supercharger after being cooled and then is recycled into the atomizing chamber through nitrogen, and the mass ratio of the metal manganese and the nitrogen entering the atomizing chamber is 9-15: 1.
further, the manganese nitride powder product is mixed with a binder, the mixture is placed in a feeding bin on a forging press or a roller press and then pressed into a manganese nitride ball or a manganese nitride pillow, the density reaches 4-5 g/cm after pressing forming, each finished product is 250-500 g in unit weight, and the finished products are packaged by a ton bag or an iron bucket after drying and solidification.
Furthermore, the drying and consolidation of the manganese nitride ball (pillow) are realized by drying with hot air or natural drying through air circulation at normal temperature.
Further, the manganese metal raw material is electrolytic manganese metal or manganese-silicon alloy or manganese-iron alloy.
Further, the pure nitrogen gas refers to a pure nitrogen gas having a nitrogen content of 99.99%.
Further, the binder is sodium water glass or potassium water glass or instant powdery sodium silicate.
Further, when the binder is made of instant powdery sodium silicate, the binder is mixed with manganese nitride powder, the mixture is placed into a feeding bin on a forging press or a roller press, water vapor is introduced into the feeding bin, the steam and the instant powdery sodium silicate are wetted by contact and have viscosity, then the mixture is pressed into manganese nitride balls or manganese nitride pillows, and the manganese nitride balls or manganese nitride pillows are naturally dried by ventilation at normal temperature to obtain manganese nitride balls or manganese nitride pillows products.
The invention has the beneficial effects that:
1. the product quality is good, the content of manganese oxide in the product is reduced, and the yield of manganese element is improved. When the metal manganese is molten, the manganese oxide on the metal manganese is removed in the form of scum, and new manganese oxide is not generated by subsequent nitridation. Manganese oxide is not easy to generate even if manganese nitride powder is re-pressed into balls, because manganese melt liquid is atomized into particles, small crystals similar to glass are formed under the protection of atmosphere, the specific surface area is small, the manganese oxide is not easy to be oxidized, in addition, liquid water glass is not used as a binder, the possibility of generating manganese oxide is greatly reduced, the oxygen content of the manganese nitride powder finished product is controlled to be below 0.5 percent, and the oxygen content of the manganese nitride ball (pillow) finished product is controlled to be below 0.8 percent and is far lower than the oxygen content of the existing product by 3 percent.
2. The superfine metal manganese powder is recycled and produced in manganese powder preparation, so that the condition that the superfine powder is too much to be utilized is avoided; the nitrogen utilization rate is high, and nitrogen which is not subjected to nitridation reaction is recycled and is not discharged.
3. The production process is short, and the manganese nitride powder can be obtained by electrolyzing the metal manganese sheet in one step. The manganese powder preparation and the nitriding are integrated, the production is easy to realize automatic control, the production efficiency is high, the environmental pollution is small, the comprehensive production cost is low, and the comprehensive power consumption can be controlled below 380 ℃ per ton of products.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The present invention will now be described by way of example with reference to FIG. 1. The device for preparing the superfine active aluminum powder by the nitrogen atomization method is modified, a gas melting furnace is changed into a medium-frequency induction melting electric furnace on the basis of the original device for preparing the superfine active aluminum powder by the nitrogen atomization method, and an atomizer connected to the upper part of an atomization chamber adopts a high-temperature resistant material; in addition add wen's duster on atomizer chamber upper portion, add wen's duster in the atomizer chamber lower part to increase the heat transfer area of the indoor water-cooled heat exchanger of atomizer, configuration blendor, forging press, measurement equipment for packing, in addition hierarchical only use second grade cyclone, reform transform the device and accomplish the back, concrete operation is as follows:
firstly, melting metal manganese sheets: putting the electrolytic manganese metal sheet into a medium-frequency induction smelting furnace, controlling the smelting temperature to 1450 ℃, and refining the molten manganese liquid to remove the upper manganese oxide slag.
Secondly, atomizing to prepare powder: introducing pure nitrogen into an atomizer, performing atmosphere replacement on an atomizing chamber, a cooler and a cyclone separator, sucking molten manganese liquid into the atomizer when the oxygen content of gas at the outlet of the cyclone separator is less than 0.5%, atomizing into small liquid drops in the atomizing chamber, introducing the pure nitrogen into a Venturi powder sprayer, spraying over-fine metal manganese powder into the atomizing chamber, colliding and adsorbing with the atomized manganese liquid drops, condensing, adjusting the temperature of the atomizing chamber by using a cooling coil and a water cooling jacket, controlling the temperature in the atomizing chamber to be 750-950 ℃, controlling the nitrogen pressure of the atomizer to be 0.8-4 MPa, and controlling the particle size of powder to be 300-500 um; controlling the nitrogen pressure of the atomizing chamber to be 0.01 MPa-0.1 MPa.
Thirdly, secondary nitridation: settling the condensed metal manganese powder to the bottom of the atomizing chamber, introducing pure nitrogen from the bottom of the atomizing chamber, performing secondary boiling nitridation on the metal manganese powder, and controlling the nitridation temperature to be 750-900 ℃.
Fourthly, cooling and packaging: after secondary nitridation, the material is cooled to normal temperature by a cooler, the material discharged from a discharge outlet of the cooler is a manganese nitride powder product, powder-containing gas at an exhaust port of the cooler enters a primary separator, and fine powder discharged from a discharge outlet of the primary separator is also used as the manganese nitride powder product.
Preferably, the powder-containing gas discharged from the exhaust port of the primary separator enters a secondary separator and then enters a dust remover, the fine powder discharged from the discharge ports of the secondary separator and the dust remover enters an atomizing chamber through a venturi powder sprayer for recycling, the tail gas at the outlet of the dust remover is cooled and then enters a supercharger for pressurizing, and then nitrogen is recycled to the atomizing chamber, and the mass ratio of the manganese metal to the nitrogen entering the atomizing chamber is 12: 1.
preferably, the manganese nitride powder product is mixed with instant powdery sodium silicate, the mixture is placed into a feeding bin on a roller press, water vapor is introduced into the feeding bin to enable the steam and the instant powdery sodium silicate to be wet in contact and have viscosity, then the mixture is pressed into manganese nitride balls, the density reaches 4-6 g/cm after the manganese nitride balls are pressed and formed, the unit weight of each finished product is 250-300 g, and the finished products are packaged by ton bags or iron barrels after natural drying through air circulation at normal temperature.
The manganese nitride powder product produced by the method is compared with the existing product in terms of power consumption.
The quality data of the manganese nitride powder produced by the method is compared with the existing product.
| Mn | N | O | Mn+N | |
| Content of existing product (%) | 87.9 | 8.8 | 2.9 | 96.7 |
| Content of inventive product (%) | 89.2 | 10.4 | 0.2 | 99.6 |
The foregoing shows and describes the general principles and features of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (8)
1. The efficient and energy-saving manganese nitride production process is characterized by comprising the following steps of:
firstly, melting metal manganese: putting a manganese metal raw material into an electromagnetic induction smelting furnace, controlling the smelting temperature to 1350-1600 ℃ to obtain molten manganese liquid, and refining the molten manganese liquid to remove upper-layer manganese oxide scum;
secondly, primary atomization nitridation: introducing pure nitrogen into an atomizer, sucking molten manganese liquid into the atomizer, atomizing into small liquid drops in an atomizing chamber, introducing pure nitrogen into a Venturi powder sprayer, sucking the fine powder into the Venturi powder sprayer, then spraying into the atomizing chamber, colliding and adsorbing with the atomized manganese liquid drops, and condensing into powder; meanwhile, the temperature of the atomizing chamber is adjusted by a cooling coil and a water cooling jacket in the atomizing chamber, the temperature in the atomizing chamber is 750-950 ℃, the nitrogen pressure of the atomizer is controlled to be 0.8-4 MPa, and the particle size of the powder is controlled to be 300-500 um; controlling the nitrogen pressure of the atomizing chamber to be 0.01 MPa-0.1 MPa;
thirdly, secondary nitridation: depositing the hot metal manganese powder to the bottom of the atomizing chamber, introducing pure nitrogen from the bottom of the atomizing chamber, performing secondary boiling nitridation on the metal manganese powder, and controlling the nitridation temperature to be 750-950 ℃;
fourthly, cooling and packaging: after secondary nitridation, the material is cooled to normal temperature by a cooler, the material discharged from a discharge port of the cooler is a manganese nitride powder product, powder-containing gas at an exhaust port of the cooler enters a primary separator, fine powder discharged from a discharge port of the primary separator is also used as the manganese nitride powder product, the powder-containing gas discharged from the exhaust port of the primary separator enters a secondary separator and then enters a dust remover, and fine powder discharged from the discharge port of the secondary separator and the discharge port of the dust remover enters an atomizing chamber for recycling through a Venturi powder sprayer.
2. The efficient and energy-saving manganese nitride production process according to claim 1, wherein tail gas at the outlet of the dust remover is cooled and then enters a supercharger for pressurization and then is recycled to the atomization chamber, and the mass ratio of metal manganese to nitrogen entering the atomization chamber is 9-15: 1.
3. an efficient and energy-saving manganese nitride production process according to claim 1, wherein the manganese metal raw material is electrolytic manganese metal or manganese silicon alloy or manganese iron alloy.
4. The process for producing manganese nitride with high efficiency and energy saving according to claim 1, wherein the pure nitrogen gas is pure nitrogen gas with 99.99% of nitrogen content.
5. The efficient and energy-saving manganese nitride production process according to claim 1, wherein the manganese nitride powder is mixed with a binder, then pressed into manganese nitride balls or manganese nitride pillows, pressed and formed, the density reaches 4-5 g/cm for double-cropping, each finished product has a single weight of 250-500 g, and the finished products are packaged by ton bags or iron drums after being dried and solidified.
6. The process for producing manganese nitride with high efficiency and energy saving according to claim 5, wherein the drying and consolidation of the manganese nitride balls formed by pressing are drying by hot air or natural drying by normal temperature air circulation.
7. A high efficiency energy saving manganese nitride production process according to claim 5, wherein said binder is sodium or potassium water glass or instant powdered sodium silicate.
8. The production process of manganese nitride according to claim 7, wherein the binder is instant powdered sodium silicate, the mixture is mixed with manganese nitride powder, the mixture is placed into a feeding bin on a forging press or a roller press, water vapor is introduced into the feeding bin to wet the steam and the instant powdered sodium silicate in a contact manner, the mixture has viscosity, the mixture is pressed into manganese nitride balls or manganese nitride pillows, and then the manganese nitride balls or manganese nitride pillows are naturally dried under normal temperature air circulation to obtain the manganese nitride balls or manganese nitride pillows.
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