CN109694982B - Preparation process of vanadium-nitrogen alloy - Google Patents
Preparation process of vanadium-nitrogen alloy Download PDFInfo
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- CN109694982B CN109694982B CN201910186719.1A CN201910186719A CN109694982B CN 109694982 B CN109694982 B CN 109694982B CN 201910186719 A CN201910186719 A CN 201910186719A CN 109694982 B CN109694982 B CN 109694982B
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Abstract
The invention discloses a preparation process of a vanadium-nitrogen alloy, and relates to the technical field of metallurgy. The preparation process of the vanadium-nitrogen alloy comprises the following steps: uniformly mixing vanadium oxide, carbonaceous reducing agent, accelerant and binder, and then pressing and forming to obtain a formed material; sintering the molding material in sections to obtain vanadium-nitrogen alloy; the segmented sintering comprises four heating sections which are sequentially and continuously carried out: the first working section, the temperature is 0-650 ℃, and the heating time is 100-120 min; the temperature of the second working section is 700-900 ℃, and the heating time is 250-280 min; in the third working section, the temperature is not lower than 1100 ℃, and the heating time is 200-220 min; the temperature of the fourth working section is 1100-1500 ℃, and the heating time is 1000-1200 min. The invention aims to analyze the reaction condition of materials during the preparation of vanadium-nitrogen alloy, perform the sintering process in sections, and strictly control the temperature and time of each section, thereby improving the quality of vanadium-nitrogen alloy products and ensuring that the prepared products have more stable quality.
Description
Technical Field
The invention relates to the technical field of metallurgy, in particular to a preparation process of a vanadium-nitrogen alloy.
Background
The vanadium-nitrogen alloy is a steel additive: the vanadium carbide or vanadium nitride precipitate can pin dislocation and grain boundary and block the dislocation and grain boundary migration, thereby improving the strength of the steel; meanwhile, the precipitation of vanadium carbonitride can be strengthened by adding nitrogen into steel, the interphase distribution of vanadium is changed, the precipitation strengthening effect of vanadium is fully exerted, and the nitrogen permeates into the steel and can refine crystal grains, so that when steel materials are produced, vanadium-nitrogen alloy is added into the steel, the crystal grains can be effectively strengthened and refined, vanadium-containing raw materials are saved, the toughness of the steel is improved, the steel has good weldability, the steel-making production cost is reduced, and the demand of the steel production on high-quality vanadium-nitrogen alloy is increased day by day.
In the current industrial production, the commonly used vanadium-nitrogen alloy preparation method is a carbothermic reduction-nitridation method, namely, raw materials such as vanadium pentoxide and the like are pressed and molded and then placed under nitrogen flow, and are subjected to rapid thermal sintering (namely direct high-temperature heating) under a high-temperature environment to prepare the vanadium-nitrogen alloy, and during the process, oxygen in the vanadium pentoxide is replaced by nitrogen.
Disclosure of Invention
The invention mainly aims to provide a preparation process of a vanadium-nitrogen alloy, aiming at improving the quality of a vanadium-nitrogen alloy product and ensuring that the quality of the prepared product is more stable.
In order to achieve the purpose, the invention provides a preparation process of a vanadium-nitrogen alloy, which comprises the following steps:
uniformly mixing vanadium oxide, carbonaceous reducing agent, accelerant and binder, and then pressing and forming to obtain a formed material;
sintering the molding material in sections to obtain vanadium-nitrogen alloy;
the segmented sintering comprises four heating sections which are sequentially and continuously carried out:
the first working section, the temperature is 0-650 ℃, and the heating time is 100-120 min;
the temperature of the second working section is 700-900 ℃, and the heating time is 250-280 min;
in the third working section, the temperature is not lower than 1100 ℃, and the heating time is 200-220 min;
the temperature of the fourth working section is 1100-1500 ℃, and the heating time is 1000-1200 min.
Preferably, in the step of obtaining the molding material, after uniformly mixing the vanadium oxide compound, the carbonaceous reducing agent, the accelerator and the binder, the vanadium oxide compound is one or a mixture of more of vanadium pentoxide, vanadium trioxide and vanadium dioxide.
Preferably, in the step of uniformly mixing the vanadium oxide compound, the carbonaceous reducing agent, the promoter and the binder, and performing compression molding to obtain a molded material, the weight ratio of the vanadium oxide compound to the carbonaceous reducing agent to the binder to the promoter is 100 (25-30): (0.4-0.8): (3-5).
Preferably, the binder is a mixture of one or more of water, starch and polyvinyl alcohol; and/or the presence of a gas in the gas,
the accelerant is one or a mixture of iron powder, ferric oxide powder and ferrous carbonate powder.
Preferably, the step of mixing the vanadium oxide compound, the carbonaceous reducing agent, the accelerator and the binder uniformly, and then performing compression molding to obtain the molding material further comprises the following steps: grinding the vanadium-oxygen compound until the grinding particle size is-150 to-120 meshes for later use.
Preferably, the step of sintering the molding material in stages to obtain the vanadium-nitrogen alloy is carried out in a nitrogen atmosphere;
wherein the volume percentage concentration of the nitrogen is not less than 99.99 percent, the pressure of the nitrogen is 0.1-0.2 MPa, and the flow rate of the nitrogen is 10-15 m3/h。
Preferably, the temperature of the third section is 1100-1250 ℃, and the heating time is 205-215 min.
Preferably, the temperature of the fourth section is 1480-1500 ℃, and the heating time is 1000-1200 min.
Preferably, the step of sintering the molding material in stages to obtain the vanadium-nitrogen alloy comprises:
sintering the molding material in sections to obtain a sintered material;
and cooling the sintered material to obtain the vanadium-nitrogen alloy, wherein the cooling temperature is not higher than 100 ℃.
In the preparation process of the vanadium-nitrogen alloy, the sintering process is carried out in sections by analyzing the reaction generated among materials during the preparation of the vanadium-nitrogen alloy, and the temperature and time of each section are strictly controlled, so that the reaction among the materials can be fully reacted step by step, the formed materials can be completely reacted from inside to outside in sequence, and the materials can be orderly and stably subjected to pollution discharge firstly and then nitrogen stabilization in the sintering process, thereby improving the quality of the vanadium-nitrogen alloy product, ensuring the prepared product to be more stable in quality, and avoiding the situations of incomplete product shrinkage or explosive cracking on the surface of the product. Moreover, the preparation method provided by the invention greatly reduces the power consumption and saves the production cost.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other related drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a process flow diagram of an embodiment of a preparation process of a vanadium-nitrogen alloy provided by the invention.
The implementation, functional features and advantages of the objects of the present invention will be further explained with reference to the accompanying drawings.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
In the current industrial production, the commonly used vanadium-nitrogen alloy preparation method is a carbothermic reduction-nitridation method, namely, raw materials such as vanadium pentoxide and the like are pressed and molded and then placed under a nitrogen flow, and are subjected to rapid thermal sintering (namely, direct heating) under a high-temperature environment to prepare the vanadium-nitrogen alloy, and during the process, oxygen in the vanadium pentoxide is replaced by nitrogen.
In view of this, the invention provides a preparation process of vanadium-nitrogen alloy, which aims to improve the quality of vanadium-nitrogen alloy products and make the quality of the prepared products more stable. With reference to the process flow diagram of an embodiment of the preparation process of the vanadium-nitrogen alloy shown in fig. 1, the preparation process of the vanadium-nitrogen alloy comprises the following steps:
and step S10, uniformly mixing the vanadium oxide compound, the carbonaceous reducing agent, the accelerant and the binder, and pressing and forming to obtain a formed material.
Wherein the vanadium-oxygen compound is one or a mixture of more of vanadium pentoxide, vanadium trioxide and vanadium dioxide; the accelerant is one or a mixture of iron powder, ferric oxide powder and ferrous carbonate powder; the binder is one or a mixture of water, starch and polyvinyl alcohol. In addition, the weight ratio of the vanadium oxide compound, the carbonaceous reducing agent, the binder and the promoter is 100 (25-30): (0.4-0.8): (3-5).
The vanadium oxide, the carbonaceous reducing agent, the accelerant and the binder are uniformly mixed, so that all reaction substances can be uniformly distributed, the formed materials can be reacted in a balanced manner at all positions, the condition that partial areas cannot react is avoided, and the quality of products is improved. Wherein, the carbonaceous reducing agent can be any one or more carbonaceous reducing agents commonly used in the metallurgical field, such as graphite, activated carbon, coke and the like; similarly, the vanadium-oxygen compound may be any one or more compounds containing vanadium and oxygen commonly used in the field of vanadium-nitrogen alloy production, but after considering the reaction and reaction products in the preparation process of the vanadium-oxygen alloy, in this embodiment, a mixture of one or more of vanadium pentoxide, vanadium trioxide and vanadium dioxide is preferred, and these three substances are all intermediate products or raw materials when vanadium pentoxide is subjected to a displacement reaction to prepare vanadium carbide or vanadium nitride, and these three substances are used as raw materials, so that the side reaction is less, the product quality is easier to control, and the vanadium content in the product is high.
In addition, in one embodiment of the present invention, before step S10, a step of activating the vanadium-oxygen compound is further included, that is:
and step S100, grinding the vanadium-oxygen compound until the grain size of the ground powder is-150 to-120 meshes for later use.
Generally speaking, the activation treatment includes physical activation and chemical activation, and the material activation treatment can enhance the reactivity of the material, in this embodiment, the present invention adopts a mechanical activation treatment manner, that is, the vanadium oxide compound is ground to a suitable particle size to increase the surface reactivity thereof, promote the reaction to proceed, further stabilize the subsequent reaction, and further improve the quality and quality stability of the product. Note that-150 to-120 mesh means that the milled powder can pass through a mesh of 150 to 120 mesh, that is, the particle size of the milled powder is smaller than the size of the mesh.
Step S20, sintering the molding material in a segmented manner to obtain vanadium-nitrogen alloy;
the segmented sintering comprises four heating sections which are sequentially and continuously carried out:
the first working section, the temperature is 0-650 ℃, and the heating time is 100-120 min;
the temperature of the second working section is 700-900 ℃, and the heating time is 250-280 min;
in the third working section, the temperature is not lower than 1100 ℃, and the heating time is 200-220 min;
the temperature of the fourth working section is 1100-1500 ℃, and the heating time is 1000-1200 min.
During the process of sintering the molding material to prepare the vanadium-nitrogen alloy, the following four reactions generally occur:
reaction 1: 2V2O5+C＝2V2O4+CO2；
Reaction 2: 2V2O4+C＝2V2O3+CO2；
Reaction 3: v2O3+5C＝2VC+3CO2；
Reaction 4: 2VC + N2＝2VN+2C。
The first reaction is an exothermic process, during which the molded material is dried and primarily carbonized, and the required temperature is not high, in the embodiment, the temperature is preferably 0-650 ℃ as the first working section heating treatment, and the heating time is preferably 100-120 min; the second reaction is a weight loss process, during which the basic pollution discharge is finished, and in the process, the temperature is not too high so as to prevent partial impurities from being discharged incompletely or the reaction is insufficient, so that in the embodiment, the temperature is strictly controlled to be 700-900 ℃, the heating time is controlled to be 250-280 min, namely, the second working section is used for completely discharging the impurities; in the third reaction, oxygen in vanadium trioxide is replaced by carbon to be changed into vanadium carbon, carbon dioxide is discharged from a smoke outlet, and multiple practices of the inventor show that during the period, when the carbonization temperature is lower than 1100 ℃, various byproducts such as metal vanadium, vanadium oxide and the like can be generated, so that the vanadium carbon cannot be completely replaced, and the conversion rate of the vanadium carbon is low, therefore, in the embodiment, as a third section, the third section is used for heating for a short time, the temperature is not lower than 1100 ℃, the heating time is 200-220 min, and in consideration of the input cost (power consumption) and the maximum income, the temperature is preferably 1100-1250 ℃, and the heating time is preferably 205-215 min. The three sections are carbonization stages, the carbonization process is carried out in sections, the temperature is gradually heated from low to high, and the technological parameters of each section are strictly controlled, so that the reaction among materials can be fully reacted step by step, and the formed materials can be completely reacted from inside to outside. In the fourth reaction, nitrogen is continuously introduced, the nitrogen replaces carbon in vanadium carbon to form vanadium nitrogen, which is an endothermic process, and by thermodynamic analysis of the nitriding process, in order to ensure that the nitriding reaction is stably and sufficiently performed, in the embodiment, the temperature of the fourth working section is 1100-1500 ℃, and preferably 1480-1500 ℃; the heating time is 1000-1200 min, preferably 1000-1200 min. The four working sections are sequentially and continuously carried out, so that heat loss can be avoided, the cost is saved, and meanwhile, the materials can be orderly and stably discharged in the sintering process and then stabilized in nitrogen, so that the quality of the vanadium-nitrogen alloy product is improved, the quality of the prepared product is more stable, and the condition that the product is not shrunk in place or the surface of the product is cracked is avoided.
In addition, in order to further maintain the stable product quality, the nitrogen protection is carried out in the reaction process, namely the reaction is carried outThe four sections are all carried out in nitrogen atmosphere to prevent the interference of outside air, which is beneficial to the stable operation of the whole reaction process. In specific implementation, the nitrogen adopted by the method is nitrogen with the volume percentage concentration of not less than 99.99 percent, the nitrogen pressure is 0.1-0.2 MPa, and the nitrogen flow rate is 10-15 m3/h。
When step S20 is implemented, this step may be implemented as the following steps:
step S210, sintering the molding material in sections to obtain a sintered material;
and S220, cooling the sintered material to obtain the vanadium-nitrogen alloy, wherein the cooling temperature is not higher than 100 ℃.
In specific implementation, the cooling step can be realized by water cooling or nitrogen cooling.
The technical solutions of the present invention are further described in detail below with reference to specific examples and drawings, it should be understood that the following examples are merely illustrative of the present invention and are not intended to limit the present invention.
Example 1
1000kg of powdery vanadium oxide (vanadium pentoxide and vanadium content of 61%) which is ground to have the milled particle size of-150 meshes, 280kg of carbonaceous reducing agent (graphite powder), 5kg of binder (water) and 40kg of accelerant (iron powder) are uniformly mixed, and then pressure is applied to form an ellipsoidal forming object with the thickness of 50mm × 50mm, 50mm and × 30 mm.
The shaped article is loaded into crucibles, and the crucibles are fed into a sintering furnace for heating, the sintering furnace being divided into four temperature zones of different temperatures, wherein the temperature of the first temperature zone is set to 650 ℃, the temperature of the second temperature zone is set to 800 ℃, the temperature of the third temperature zone is set to 1100 ℃, and the temperature of the fourth temperature zone is set to 1500 ℃. Introducing nitrogen into the crucible to ensure that the formed product in the crucible is in a nitrogen atmosphere (the volume percentage concentration of the nitrogen is not less than 99.99 percent, the nitrogen pressure is 0.2MP, and the nitrogen flow rate is 15 m)3H) carrying out heating reaction in the first temperature zone, the second temperature zone, the third temperature zone and the fourth temperature zone in sequence. By controlling the moving speed of the push plate inside, the residence time of the crucible in the first temperature zone is 100min and 260min,the residence time in the first temperature zone is 210min, and the residence time in the first temperature zone is 1000 min. And then introducing nitrogen at room temperature into the furnace for cooling, and obtaining a high-quality vanadium-nitrogen alloy product after the materials in the crucible are cooled to be below 100 ℃.
Example 2
1000kg of powdery vanadium oxide (vanadium trioxide, with the vanadium content of 55.4%) which is ground to the powder size of-150 meshes, 250kg of carbonaceous reducing agent (graphite powder), 4kg of binder (starch) and 30kg of accelerant (ferrous carbonate powder) are uniformly mixed, and then pressure is applied to form an ellipsoidal forming object with the grain size of 50mm × 50mm, 50mm and × 30 mm.
The shaped article is charged into crucibles, and the crucibles are fed into a sintering furnace for heating, the sintering furnace being divided into four temperature zones of different temperatures, wherein the temperature of the first temperature zone is set to 630 ℃, the temperature of the second temperature zone is set to 850 ℃, the temperature of the third temperature zone is set to 1200 ℃, and the temperature of the fourth temperature zone is set to 1495 ℃. Introducing nitrogen into the crucible to ensure that the formed product in the crucible is in a nitrogen atmosphere (the volume percentage concentration of the nitrogen is not less than 99.99 percent, the nitrogen pressure is 0.1MP, and the nitrogen flow rate is 13 m)3H) carrying out heating reaction in the first temperature zone, the second temperature zone, the third temperature zone and the fourth temperature zone in sequence. By controlling the moving speed of the push plate, the residence time of the crucible in the first temperature zone is 105min, the residence time in the first temperature zone is 280min, the residence time in the first temperature zone is 205min, and the residence time in the first temperature zone is 1100 min. And then introducing nitrogen at room temperature into the furnace for cooling, and obtaining a high-quality vanadium-nitrogen alloy product after the materials in the crucible are cooled to be below 100 ℃.
Example 3
1000kg of powdery vanadium oxide (vanadium dioxide, vanadium content 67%) which is ground to have the powder size of-120 meshes, 300kg of carbonaceous reducing agent (coke powder), 8kg of adhesive (polyvinyl alcohol) and 50kg of accelerant (ferroferric oxide powder) are uniformly mixed, and then pressure is applied to form an ellipsoidal forming object with the thickness of 50mm × 50mm, 50mm and × 30 mm.
The shaped bodies are placed in crucibles and the crucibles are heated in a sintering furnace which is divided into four temperature zones of different temperaturesWherein, the temperature of the first temperature zone is set to 580 ℃, the temperature of the second temperature zone is set to 750 ℃, the temperature of the third temperature zone is set to 1150 ℃, and the temperature of the fourth temperature zone is set to 1490 ℃. Introducing nitrogen into the crucible to ensure that the formed product in the crucible is in a nitrogen atmosphere (the volume percentage concentration of the nitrogen is not less than 99.99 percent, the nitrogen pressure is 0.2MP, and the nitrogen flow rate is 12 m)3H) carrying out heating reaction in the first temperature zone, the second temperature zone, the third temperature zone and the fourth temperature zone in sequence. By controlling the moving speed of the push plate inside, the residence time of the crucible in the first temperature zone is 105min, 250min, 200min and 1200 min. And then introducing nitrogen at room temperature into the furnace for cooling, and obtaining a high-quality vanadium-nitrogen alloy product after the materials in the crucible are cooled to be below 100 ℃.
Example 4
1000kg of powdery vanadium oxide compounds (vanadium pentoxide and vanadium trioxide, with the vanadium content of 67.3%) which are ground to the powder size of-140 meshes, 260kg of carbonaceous reducing agent (activated carbon), 7kg of binding agent (aqueous solution of polyvinyl alcohol) and 45kg of accelerant (iron powder and ferroferric oxide powder) are uniformly mixed, and then pressure is applied to form an ellipsoidal forming object with the grain size of 50mm × 50mm, 50mm and × 30 mm.
The shaped article is loaded into crucibles, and the crucibles are fed into a sintering furnace for heating, the sintering furnace is divided into four temperature zones of different temperatures, wherein the temperature of the first temperature zone is set to 560 ℃, the temperature of the second temperature zone is set to 700 ℃, the temperature of the third temperature zone is set to 1250 ℃, and the temperature of the fourth temperature zone is set to 1480 ℃. Introducing nitrogen into the crucible to ensure that the formed product in the crucible is in a nitrogen atmosphere (the volume percentage concentration of the nitrogen is not less than 99.99 percent, the nitrogen pressure is 0.15MP, and the nitrogen flow rate is 10 m)3H) carrying out heating reaction in the first temperature zone, the second temperature zone, the third temperature zone and the fourth temperature zone in sequence. By controlling the moving speed of the push plate inside, the residence time of the crucible in the first temperature zone is 110min, 270min, 220min and 1150 min. Then, nitrogen gas at room temperature is introduced into the furnaceAnd cooling, namely cooling the materials in the crucible to be below 100 ℃ to obtain the high-quality vanadium-nitrogen alloy product.
Example 5
1000kg of powdery vanadium oxide compound (vanadium trioxide and vanadium dioxide, the vanadium content of which is 49.6%) ground to-130 meshes, 290kg of carbonaceous reducing agent (graphite powder), 6kg of binder (aqueous solution of starch) and 35kg of accelerant (mixture of iron powder, ferroferric oxide powder and ferrous carbonate powder) are uniformly mixed, and then pressure is applied to form an ellipsoidal forming object with the grain size of 50mm × 50mm, 50mm and × 30 mm.
The shaped article is charged into crucibles, and the crucibles are fed into a sintering furnace for heating, the sintering furnace being divided into four temperature zones of different temperatures, wherein the temperature of the first temperature zone is set to 450 ℃, the temperature of the second temperature zone is set to 900 ℃, the temperature of the third temperature zone is set to 1350 ℃, and the temperature of the fourth temperature zone is set to 1100 ℃. Introducing nitrogen into the crucible to ensure that the formed product in the crucible is in a nitrogen atmosphere (the volume percentage concentration of the nitrogen is not less than 99.99 percent, the nitrogen pressure is 0.12MP, and the nitrogen flow rate is 11 m)3H) carrying out heating reaction in the first temperature zone, the second temperature zone, the third temperature zone and the fourth temperature zone in sequence. By controlling the moving speed of the push plate, the residence time of the crucible in the first temperature zone is 115min, 260min, 215min and 1000 min. And then introducing nitrogen at room temperature into the furnace for cooling, and obtaining a high-quality vanadium-nitrogen alloy product after the materials in the crucible are cooled to be below 100 ℃.
Example 6
1000kg of powdery vanadium oxide (vanadium pentoxide and vanadium content of 61%) which is ground to have the powder size of-120 meshes, 270kg of carbonaceous reducing agent (graphite powder), 4.7kg of binder (water) and 48kg of accelerant (iron powder) are uniformly mixed, and then pressure is applied to form an ellipsoidal forming object with the thickness of 50mm × 50mm, 50mm × 30 mm.
Loading the formed object into crucibles, and heating the crucibles in a sintering furnace divided into four temperature zones of different temperatures, wherein the temperature of the first temperature zone is set to 300 ℃ and the temperature of the second temperature zone is set to 300 ℃The temperature of the third temperature zone was set to 800 deg.C, the temperature of the third temperature zone was set to 1450 deg.C, and the temperature of the fourth temperature zone was set to 1200 deg.C. Introducing nitrogen into the crucible to ensure that the formed product in the crucible is in a nitrogen atmosphere (the volume percentage concentration of the nitrogen is not less than 99.99 percent, the nitrogen pressure is 0.18MP, and the nitrogen flow rate is 14 m)3H) carrying out heating reaction in the first temperature zone, the second temperature zone, the third temperature zone and the fourth temperature zone in sequence. By controlling the moving speed of the push plate, the residence time of the crucible in the first temperature zone is 120min, 265min, 210min and 1010 min. And then introducing nitrogen at room temperature into the furnace for cooling, and obtaining a high-quality vanadium-nitrogen alloy product after the materials in the crucible are cooled to be below 100 ℃.
Comparative example
1000kg of powdery vanadium pentoxide (containing 61 percent of vanadium), 200kg of graphite powder, 25kg of iron powder and 140kg of 3 percent polyvinyl alcohol aqueous solution are uniformly mixed, then pressure is applied to form ellipsoidal forming objects with the thickness of 50mm × 50mm × 30mm, the forming objects are put into crucibles, the crucibles are fed into a sintering furnace to be heated, firstly, carbonization reaction is carried out at 1450 ℃ is carried out for 5 hours, then nitridation reaction is carried out at 1000 ℃ for 1.5 hours, nitrogen is introduced during the process, then, nitrogen at room temperature is introduced into the furnace to be cooled, and after materials in the crucibles are cooled to below 150 ℃, vanadium-nitrogen alloy products can be obtained.
The above examples and comparative examples were tested, and the test items include the appearance quality of the vanadium-nitrogen alloy product (the percentage of the total output of the high-quality product with good surface quality, no cracking and uniform specific gravity), the nitrogen content, the vanadium content, the apparent density and the power consumption in production. The recorded data are shown in tables 1 and 2 below.
TABLE 1 product quality testing
TABLE 2 comparison of Power consumption
As can be seen from Table 1, the vanadium and nitrogen contents and the apparent density of the vanadium-nitrogen alloy prepared in each example are close to those of the comparative example, and the vanadium-nitrogen alloy meets the national standard of GB/T20567-2006 vanadium-nitrogen alloy. However, the ratio of the high-quality products is obviously higher than that of the comparative examples, which shows that the preparation process of the vanadium-nitrogen alloy provided by the invention overcomes the defects of unstable product quality, easy surface cracking and product shrinkage failure (uneven specific gravity) of the products prepared by the existing method, namely, the products prepared by the preparation method provided by the invention have high quality and high quality stability. As can be seen from Table 2, the power consumption of the production of each example is significantly lower than that of the comparative example, which shows that the preparation process of the vanadium-nitrogen alloy provided by the invention has low power consumption and low production cost.
The above is only a preferred embodiment of the present invention, and it is not intended to limit the scope of the invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention shall be included in the scope of the present invention.
Claims (8)
1. The preparation process of the vanadium-nitrogen alloy is characterized by comprising the following steps of:
uniformly mixing vanadium oxide, carbonaceous reducing agent, accelerant and binder, and then pressing and forming to obtain a formed material;
sintering the molding material in sections to obtain vanadium-nitrogen alloy;
the segmented sintering comprises four heating sections which are sequentially and continuously carried out:
the first working section, the temperature is 0-650 ℃, and the heating time is 100-120 min;
the temperature of the second working section is 700-900 ℃, and the heating time is 250-280 min;
the temperature of the third section is 1100-1250 ℃, and the heating time is 205-215 min;
the temperature of the fourth working section is 1100-1500 ℃, and the heating time is 1000-1200 min.
2. The process for preparing the vanadium-nitrogen alloy according to claim 1, wherein in the step of obtaining the molding material by uniformly mixing a vanadium-oxygen compound, a carbonaceous reducing agent, a promoter and a binder, and then performing compression molding, the vanadium-oxygen compound is one or more of vanadium pentoxide, vanadium trioxide and vanadium dioxide.
3. The preparation process of the vanadium-nitrogen alloy as claimed in claim 1, wherein in the step of obtaining the molding material by uniformly mixing the vanadium oxide compound, the carbonaceous reducing agent, the promoter and the binder, and then performing compression molding, the weight ratio of the vanadium oxide compound, the carbonaceous reducing agent, the binder and the promoter is 100 (25-30): (0.4-0.8): (3-5).
4. The process for preparing the vanadium-nitrogen alloy according to claim 3, wherein the binder is a mixture of one or more of water, starch and polyvinyl alcohol; and/or the presence of a gas in the gas,
the accelerant is one or a mixture of iron powder, ferric oxide powder and ferrous carbonate powder.
5. The process for preparing a vanadium-nitrogen alloy according to claim 1, wherein the step of mixing the vanadium oxide compound, the carbonaceous reducing agent, the accelerator and the binder, and then press-forming the mixture to obtain a formed material further comprises the steps of: grinding the vanadium-oxygen compound until the grinding particle size is-150 to-120 meshes for later use.
6. The process for preparing a vanadium-nitrogen alloy according to claim 1, wherein the step of sintering the molding material in stages to obtain the vanadium-nitrogen alloy is performed in a nitrogen atmosphere;
wherein the volume percentage concentration of the nitrogen is not less than 99.99%, the pressure of the nitrogen is 0.1-0.2 MPa, and the nitrogen flowsThe speed is 10-15 m3/h。
7. The preparation process of the vanadium-nitrogen alloy as claimed in claim 1, wherein the temperature of the fourth section is 1480 to 1500 ℃ and the heating time is 1000 to 1200 min.
8. The process for preparing the vanadium-nitrogen alloy as claimed in claim 1, wherein the step of sintering the molding material in stages to obtain the vanadium-nitrogen alloy comprises:
sintering the molding material in sections to obtain a sintered material;
and cooling the sintered material to obtain the vanadium-nitrogen alloy, wherein the cooling temperature is not higher than 100 ℃.
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| CN111485159B (en) * | 2020-05-26 | 2021-09-10 | 江苏中钒新材料科技有限公司 | Preparation method of vanadium-nitrogen alloy |
| CN112301247A (en) * | 2020-10-15 | 2021-02-02 | 天津炜润达新材料科技有限公司 | Method for preparing vanadium nitride from vanadium slag |
| CN113718105A (en) * | 2021-08-30 | 2021-11-30 | 攀钢集团钒钛资源股份有限公司 | With V2O5Method for efficiently preparing vanadium-nitrogen alloy for heat booster |
| CN115259163B (en) * | 2022-07-19 | 2023-10-10 | 宁波合盛新材料有限公司 | Synthesis method of cerium silicide |
| CN115821140B (en) * | 2022-11-24 | 2024-04-30 | 河南融发新材料科技有限公司 | Titanium-containing alloy for metallurgy and low-cost production method thereof |
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