CN109097563B - Preparation method of vanadium-nitrogen alloy - Google Patents
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Abstract
The invention relates to a preparation method of vanadium-nitrogen alloy, belonging to the technical field of preparation of iron alloy. The invention aims to solve the problem that the vanadium content of vanadium-nitrogen alloy continuously prepared by the existing pushed slab kiln fluctuates greatly, the technical scheme is to provide a preparation method of the vanadium-nitrogen alloy, the preparation raw material comprises vanadium oxide, carbonaceous powder, iron powder and a binder, wherein the addition amount of the iron powder is controlled according to the following percentage relationship: the mass of iron powder/theoretical yield of vanadium-nitrogen alloy is 80% -the target content of vanadium in vanadium-nitrogen alloy-the total mass of Si, Fe, Mn, Cr and Al in vanadium oxide/theoretical yield of vanadium-nitrogen alloy is 100%. The preparation method has the advantages of small vanadium-nitrogen content fluctuation, low oxygen content and high density of the obtained product.
Description
Technical Field
The invention relates to a preparation method of vanadium-nitrogen alloy, belonging to the technical field of preparation of iron alloy.
Background
The vanadium-nitrogen alloy is an important vanadium alloy additive, and can be added into steel to improve the comprehensive mechanical properties of the steel, such as wear resistance, corrosion resistance, toughness, strength, ductility, hardness, fatigue resistance and the like, and ensure that the steel has good weldability. Particularly in high-strength low alloy steel, microalloy steel and other special steel, the vanadium-nitrogen alloy can effectively strengthen and refine grains, and saves vanadium-containing raw materials, thereby reducing the steelmaking production cost. Research shows that after nitrogen is added into vanadium steel, vanadium in a solid solution state is converted into vanadium in a precipitation state, so that the quantity of V (CN) precipitation phases is multiplied, and the precipitation strengthening effect of vanadium is fully exerted.
At present, the method for producing vanadium-nitrogen alloy mainly comprises the steps of continuously preparing vanadium-nitrogen alloy by a pushed slab kiln, preparing vanadium-nitrogen alloy by a microwave oven and preparing vanadium-nitrogen alloy by a rotary kiln. Wherein, the process for preparing the vanadium-nitrogen alloy by the microwave oven and the rotary kiln is not mature, and does not have industrialized production conditions; in the method for continuously preparing the vanadium-nitrogen alloy by the pushed slab kiln, the vanadium content (70-81%), the nitrogen content (12-18%) and other contents of the product have large fluctuation, the oxygen content is higher (more than 1.2%), and the strengthening effect of the vanadium-nitrogen alloy in steel is influenced. For example, CN101392333A provides a method for preparing a vanadium-nitrogen alloy: the raw material is vanadium pentoxide or vanadium trioxide, carbonaceous catalyst or graphite, 97.7-72.7 wt% of vanadium pentoxide or vanadium trioxide and 27.3-2.3 wt% of carbonaceous catalyst or graphite are uniformly mixed, and then the mixture is made into spherical material by using high-pressure ball machine, and in the medium-frequency induction furnace, the temperature is raised to 1200 ℃ in nitrogen-containing irregular original atmosphere for 1350 deg.C, and the mixture is reduced for 2.5-3.5 h. The vanadium-nitrogen alloy prepared by the method has the defects of large fluctuation of vanadium-nitrogen content and over high oxygen content, wherein the vanadium content is 70.1-78.4%, the nitrogen content is 12.6-18.2%, and the oxygen content is 1.9-2.0%.
Disclosure of Invention
The invention aims to provide a preparation method of vanadium-nitrogen alloy, which aims to solve the problem that the vanadium content of the vanadium-nitrogen alloy continuously prepared by the existing pushed slab kiln fluctuates greatly. The invention also aims to solve the problems of large nitrogen content fluctuation and overhigh oxygen content in the vanadium-nitrogen alloy.
The invention provides a preparation method of vanadium-nitrogen alloy, which comprises the following steps of preparing raw materials comprising vanadium oxide, carbonaceous powder, iron powder and a binder, wherein the addition amount of the iron powder is controlled according to the following percentage relationship: the mass of iron powder/theoretical yield of vanadium-nitrogen alloy is 80% -the target content of vanadium in vanadium-nitrogen alloy-the total mass of Si, Fe, Mn, Cr and Al in vanadium oxide/theoretical yield of vanadium-nitrogen alloy is 100%.
In actual production, the theoretical yield of the vanadium-nitrogen alloy can be calculated according to the dosage of the raw material vanadium oxide, and theoretically, 1.2 parts of vanadium oxide can be prepared to obtain 1 part of vanadium-nitrogen alloy.
Further, the weight ratio of the raw materials is as follows: 100 parts of vanadium oxide, 20-30 parts of carbonaceous powder, 0.6-2.0 parts of iron powder and 5-10 parts of binder.
The addition amount of the carbonaceous powder is the theoretical amount of the reducing agent obtained according to the oxygen content in the vanadium oxide, and the residual carbon content of the vanadium-nitrogen alloy. The residual carbon content in the vanadium-nitrogen alloy before preparation is a fixed value according to the mass design, and is generally between 0.8 and 3.0. The addition amount of the carbonaceous powder is adjusted according to the oxygen content of the vanadium oxide raw material, which is beneficial to fully reducing the oxygen content in the product.
Preferably, the raw material comprises 25-28 parts of carbonaceous powder.
Preferably, the raw material comprises 0.8-1.6 parts of iron powder.
Preferably, the raw material comprises 6-8 parts of a binder.
Further, the vanadium oxide is selected from VO and VO2、V2O3、V2O5One or more than two of them.
Further, the carbonaceous powder is selected from graphite, carbon black or mixtures thereof.
Further, the binder is selected from one or more of water, starch and polyvinyl alcohol.
Furthermore, the particle size of the iron powder is-140 to-80 meshes.
Further, the vanadium content of the vanadium-nitrogen alloy is 77.3-77.5%.
Further, the nitrogen content of the vanadium-nitrogen alloy is 17.5-20%.
Further, the oxygen content of the vanadium-nitrogen alloy is < 0.5%.
Further, the apparent density of the vanadium-nitrogen alloy is more than or equal to 3.5g/cm3。
Further, the preparation method comprises the following steps: taking the raw materials in the weight ratio, uniformly mixing, carrying out pressure forming and drying to obtain a formed object, heating the formed object in a nitrogen atmosphere, and cooling to obtain the product.
Further, the temperature of the heating step is increased from 400 ℃ to 1550 ℃.
Further, the heating step comprises a preheating section, a transition section and a nitriding and sintering section, wherein the temperature of the preheating section is gradually increased from 400 ℃ to 800 ℃, and the heating time is 4-8 hours; the temperature of the transition section is increased from 800 ℃ to 1200 ℃, and the heating time is 5-8 hours; the temperature of the nitriding sintering section is increased from 1200 ℃ to 1550 ℃, and the heating time is 10-16 hours.
Preferably, the heating time of the preheating section is 5-6 hours.
Preferably, the heating time of the transition section is 5-7 hours.
Preferably, the heating time of the nitriding sintering section is 14-15 hours.
Further, the pressure of the pressure forming is 9-11 MPa.
Further, the drying temperature is 180-200 ℃.
Further, the nitrogen pressure is more than or equal to 0.3 MPa.
Further, the molded product is heated in a pusher kiln.
Further cooling to a temperature of less than or equal to 150 ℃ and discharging from the kiln.
Preferably, cooling to a temperature of less than or equal to 100 ℃ and discharging from the kiln.
The invention provides a preparation method of vanadium-nitrogen alloy, which can prepare vanadium with the content of 77.3-77.5%, nitrogen with the content of 17.5-20%, oxygen with the content of less than 0.5%, and apparent density with the density of more than 3.5g/cm3The vanadium-nitrogen alloy has the advantages of small vanadium-nitrogen content fluctuation, low oxygen content and high density of the obtained product. In addition, the preparation method can be completed under normal pressure without being implemented under vacuum condition, thereby simplifying the operation process, reducing the requirement on equipment and having popularization and application values.
Detailed Description
The raw materials and equipment used in the embodiment of the present invention are known products and obtained by purchasing commercially available products.
The invention provides a preparation method of vanadium-nitrogen alloy, which comprises the following steps of preparing raw materials comprising vanadium oxide, carbonaceous powder, iron powder and a binder, wherein the addition amount of the iron powder is controlled according to the following percentage relationship: the mass of iron powder/theoretical yield of vanadium-nitrogen alloy is 80% -the target content of vanadium in vanadium-nitrogen alloy-the total mass of Si, Fe, Mn, Cr and Al in vanadium oxide/theoretical yield of vanadium-nitrogen alloy is 100%.
The key point of the preparation method is that the aim of accurately controlling the content of vanadium in the vanadium-nitrogen alloy is achieved by adjusting the addition amount of the iron powder. The inventor finds that in the production practice, when vanadium-nitrogen alloy is prepared by taking vanadium oxide as a raw material, the fluctuation range of the content of (N + C)% in the product is small, and the content is almost constant to 20%. In addition, because the catalyst iron powder remains in the alloy after the reaction, the sum of the content of vanadium + nitrogen + carbon + iron powder + the content of vanadium oxide-introduced impurity elements Si + Fe + Mn + Cr + Al in the alloy is 100%. Based on the method, according to the amount of impurity elements sigma (Si + Fe + Mn + Cr + Al) introduced by the raw material vanadium oxide, the aim of accurately controlling the vanadium content in the vanadium-nitrogen alloy can be achieved by adjusting the addition amount of the iron powder, so that the problem of large vanadium content fluctuation in the product caused by uneven raw material vanadium oxide grades is solved.
Furthermore, the invention optimizes carbonization and nitridation effects by adjusting the technological parameters of the preheating section, the transition section and the nitridation sintering section. Wherein, the heating temperature of the preheating section is controlled to be increased from 400 ℃ to 800 ℃, so that the water and volatile gas in the material block are rapidly removed, and conditions are created for carbonization and nitridation reactions; the heating temperature of the transition section is controlled to be increased from 800 ℃ to 1200 ℃ so as to fully carry out carbonization reaction; the heating temperature of the nitriding sintering section is controlled to be increased from 1200 ℃ to 1550 ℃, and the nitriding effect is ensured to be optimal. Wherein the heating time of the preheating section is 4-8 hours, and preferably 5-6 hours according to the boiling points of water vapor, CO and CO2 and the distribution of the atmosphere in the pushed slab kiln in the production process of the vanadium-nitrogen alloy; the heating time of the transition section is 5-8 hours, and the preferable time is 5-7 hours according to the coupling process of carbonitriding in the vanadium-nitrogen alloy reaction process; the heating time of the nitriding sintering section is 10 to 16 hours, and preferably 14 to 15 hours according to the mechanism of the nitriding reaction.
By optimizing the process parameters of the preheating section, the transition section and the nitriding and sintering section, the following benefits can be brought: 1. improving the nitrogen content in the vanadium-nitrogen alloy, and accurately controlling the nitrogen content in the product to be 17.5-20%; 2. the oxygen content of the vanadium-nitrogen alloy is fully reduced; 3. the apparent density of the product is improved.
In the following examples, the nitrogen content, vanadium content, oxygen content and apparent density of the vanadium-nitrogen alloy product were measured according to the method of GB/T20567-2006.
Example 1 preparation of vanadium-nitrogen alloy by the method of the invention
100 parts of vanadium trioxide (containing 61 percent of vanadium, sigma (Si + Fe + Mn + Cr + Al) ═ 1.2 percent), 28 parts of graphite powder and 1.0 part of iron powder are uniformly mixed, 6 percent of binder (water) is added, then wet mixing is carried out for 30 minutes, and 9MPa pressure is applied to form the mixture into 50mm multiplied by 30mm ellipsoidal forming shapeThe shaped material is dried in crucible at 180 deg.c for 14 hr, and the crucible is fed into double pushing plate kiln, which is divided into preheating section, transition section, nitriding and sintering section and cooling section based on different temperature distribution inside the double pushing plate kiln. And introducing nitrogen into the crucible, so that the formed object in the crucible is subjected to heating reaction in the preheating section, the transition section and the nitriding sintering section in sequence under the nitrogen atmosphere (the nitrogen partial pressure is 0.3MP), wherein the temperature of the preheating section is 400-800 ℃, the heating temperature of the transition section is 800-1200 ℃, the heating temperature of the nitriding sintering section is 1200-1550 ℃, and the temperatures in the preheating section, the transition section and the nitriding sintering section are increased gradually along the moving direction of the crucible. The residence time of the crucible in the preheating section is 6 hours, the residence time in the transition section is 7 hours, and the residence time in the nitriding and sintering section is 15 hours by controlling the moving speed of the push plate inside. Then, the materials are sequentially subjected to nitrogen cooling for 2 hours (realized by introducing nitrogen at room temperature into the push plate type tunnel kiln) and water cooling for 2 hours (realized by arranging a water cooling jacket on a shell at the rear end of the nitrogen cooling section) in a cooling section, and the materials in the crucible are cooled to be below 100 ℃, so that a high-quality vanadium-nitrogen alloy product is obtained, wherein the vanadium-nitrogen alloy product has the nitrogen content of 17.8 wt%, the vanadium content of 77.42 wt%, the oxygen content of 0.35 wt% and the apparent density of 3.5g/cm3。
Example 2 preparation of vanadium-nitrogen alloy by the method of the invention
100 parts of vanadium trioxide (containing 62 percent of vanadium, sigma (Si + Fe + Mn + Cr + Al) is 1.0 percent), 28 parts of graphite powder and 1.2 parts of iron powder are uniformly mixed, 7 percent of binder (water) is added, then the mixture is wet-mixed for 30 minutes, 9MPa pressure is applied to form 50mm multiplied by 30mm ellipsoidal formed objects, the formed objects are put into a crucible and dried for 14 hours at the temperature of 180 ℃, the crucible is sent into a double push plate kiln, and the double push plate kiln is divided into a preheating section, a transition section, a nitriding sintering section and a cooling section according to different temperature distribution conditions in the double push plate kiln. Introducing nitrogen into the crucible to ensure that the formed object in the crucible is subjected to heating reaction in the preheating section, the transition section and the nitriding sintering section in turn under the nitrogen atmosphere (the nitrogen partial pressure is 0.3MP), thereby obtaining the productThe temperature of the preheating section is 400-800 ℃, the heating temperature of the transition section is 800-1200 ℃, the heating temperature of the nitriding sintering section is 1200-1550 ℃, and the temperatures in the preheating section, the transition section and the nitriding sintering section are respectively increased along the moving direction of the crucible. The residence time of the crucible in the preheating section is 6 hours, the residence time in the transition section is 7 hours, and the residence time in the nitriding and sintering section is 15 hours by controlling the moving speed of the push plate inside. Then, the materials are sequentially subjected to nitrogen cooling for 2 hours (realized by introducing nitrogen at room temperature into the push plate type tunnel kiln) and water cooling for 2 hours (realized by arranging a water cooling jacket on a shell at the rear end of the nitrogen cooling section) in a cooling section, and the materials in the crucible are cooled to be below 100 ℃, so that a high-quality vanadium-nitrogen alloy product is obtained, wherein the vanadium-nitrogen alloy product has the nitrogen content of 18.5 wt%, the vanadium content of 77.43 wt%, the oxygen content of 0.39 wt% and the apparent density of 3.5g/cm3。
Example 3 preparation of vanadium-nitrogen alloy by the method of the invention
100 parts of vanadium trioxide (containing 64 percent of vanadium, sigma (Si + Fe + Mn + Cr + Al) ═ 0.5 percent), 25 parts of graphite powder and 1.5 parts of iron powder are uniformly mixed, 8 percent of binder (water) is added, then the mixture is wet-mixed for 30 minutes, 9MPa pressure is applied to form 50mm multiplied by 30mm ellipsoidal formed objects, the formed objects are put into a crucible and dried for 14 hours at the temperature of 180 ℃, the crucible is sent into a double push plate kiln, and the double push plate kiln is divided into a preheating section, a transition section, a nitriding sintering section and a cooling section according to different temperature distribution conditions in the double push plate kiln. And introducing nitrogen into the crucible, so that the formed object in the crucible is subjected to heating reaction in the preheating section, the transition section and the nitriding sintering section in sequence under the nitrogen atmosphere (the nitrogen partial pressure is 0.3MP), wherein the temperature of the preheating section is 400-800 ℃, the heating temperature of the transition section is 800-1200 ℃, the heating temperature of the nitriding sintering section is 1200-1550 ℃, and the temperatures in the preheating section, the transition section and the nitriding sintering section are increased gradually along the moving direction of the crucible. The residence time of the crucible in the preheating section is 6 hours, the residence time in the transition section is 7 hours, and the residence time in the nitriding and sintering section is controlled by controlling the moving speed of the push plate insideThe residence time was 15 hours. Then, the materials are sequentially subjected to nitrogen cooling for 2 hours (realized by introducing nitrogen at room temperature into the push plate type tunnel kiln) and water cooling for 2 hours (realized by arranging a water cooling jacket on a shell at the rear end of the nitrogen cooling section) in a cooling section, and the materials in the crucible are cooled to be below 100 ℃, so that a high-quality vanadium-nitrogen alloy product is obtained, wherein the vanadium-nitrogen alloy product has the nitrogen content of 19.2 wt%, the vanadium content of 77.45 wt%, the oxygen content of 0.42 wt% and the apparent density of 3.5g/cm3。
Example 4 preparation of vanadium-nitrogen alloy by the method of the invention
100 parts of vanadium trioxide (containing 63.3 percent of vanadium, sigma (Si + Fe + Mn + Cr + Al) ═ 1.4 percent), 26.5 parts of graphite powder and 0.8 part of iron powder are uniformly mixed, 7.5 percent of binder (water) is added, then the mixture is wet-mixed for 30 minutes, 9MPa pressure is applied to the mixture to form 50mm multiplied by 30mm ellipsoidal formed objects, the formed objects are put into a crucible and dried for 14 hours at the temperature of 180 ℃, the crucible is sent into a double push plate kiln, and the double push plate kiln is divided into a preheating section, a transition section, a nitriding sintering section and a cooling section according to different temperature distribution conditions in the double push plate kiln. And introducing nitrogen into the crucible, so that the formed object in the crucible is subjected to heating reaction in the preheating section, the transition section and the nitriding sintering section in sequence under the nitrogen atmosphere (the nitrogen partial pressure is 0.3MP), wherein the temperature of the preheating section is 400-800 ℃, the heating temperature of the transition section is 800-1200 ℃, the heating temperature of the nitriding sintering section is 1200-1550 ℃, and the temperatures in the preheating section, the transition section and the nitriding sintering section are increased gradually along the moving direction of the crucible. The residence time of the crucible in the preheating section is 6 hours, the residence time in the transition section is 7 hours, and the residence time in the nitriding and sintering section is 15 hours by controlling the moving speed of the push plate inside. Then, the materials are sequentially subjected to nitrogen cooling for 2 hours (realized by introducing nitrogen at room temperature into the push plate type tunnel kiln) and water cooling for 2 hours (realized by arranging a water cooling jacket on a shell at the rear end of the nitrogen cooling section) in a cooling section, and the materials in the crucible are cooled to be below 100 ℃, so that a high-quality vanadium-nitrogen alloy product is obtained, wherein the vanadium-nitrogen alloy product has the nitrogen content of 18.7 wt%, the vanadium content of 77.42 wt%, and the oxygen content ofThe content was 0.45% by weight, and the apparent density was 3.5g/cm3。
Claims (14)
1. The preparation method of the vanadium-nitrogen alloy is characterized by comprising the following steps: the preparation method comprises the following steps of preparing raw materials comprising vanadium oxide, carbonaceous powder, iron powder and a binder, wherein the addition amount of the iron powder is controlled according to the following percentage relationship: the mass of iron powder/theoretical yield of vanadium-nitrogen alloy is 80 percent per 100 percent, the target content of vanadium in vanadium-nitrogen alloy is 80 percent per the total mass of Si, Fe, Mn, Cr and Al in vanadium oxide per the theoretical yield of vanadium-nitrogen alloy is 100 percent per the theoretical yield of vanadium-nitrogen alloy; the vanadium content of the vanadium-nitrogen alloy is 77.42-77.45%; the nitrogen content of the vanadium-nitrogen alloy is 17.5-20%; oxygen content of the vanadium-nitrogen alloy<0.5 percent; the apparent density of the vanadium-nitrogen alloy is more than or equal to 3.5g/cm3(ii) a The preparation method of the vanadium-nitrogen alloy comprises the following steps: taking raw materials in each weight ratio, uniformly mixing, pressing, forming and drying to obtain a formed object, heating the formed object in a nitrogen atmosphere, and cooling to obtain the product; the temperature of the heating step is increased from 400 ℃ to 1550 ℃; the heating step comprises a preheating section, a transition section and a nitriding and sintering section, wherein the temperature of the preheating section is increased from 400 ℃ to 800 ℃, and the heating time is 4-8 hours; the temperature of the transition section is increased from 800 ℃ to 1200 ℃, and the heating time is 5-8 hours; the temperature of the nitriding sintering section is increased from 1200 ℃ to 1550 ℃, and the heating time is 10-16 hours.
2. The method of claim 1, wherein: at least one of the following is satisfied:
the weight ratio of the raw materials is as follows: 100 parts of vanadium oxide, 20-30 parts of carbonaceous powder, 0.6-2.0 parts of iron powder and 5-10 parts of binder;
the vanadium oxide is selected from VO and VO2、V2O3、V2O5One or more than two of the components;
the carbonaceous powder is selected from graphite, carbon black or a mixture thereof;
the binder is selected from one or more of water, starch and polyvinyl alcohol;
the granularity of the iron powder is-140 to-80 meshes.
3. The method of claim 2, wherein: the raw material comprises 25-28 parts of carbonaceous powder.
4. The method of claim 2, wherein: the raw materials comprise 0.8-1.6 parts of iron powder.
5. The method of claim 2, wherein: the raw materials comprise 6-8 parts of binder.
6. The method of claim 1, wherein: the heating time of the preheating section is 5-6 hours.
7. The method of claim 1, wherein: the heating time of the transition section is 5-7 hours.
8. The method of claim 1, wherein: the heating time of the nitriding sintering section is 14-15 hours.
9. The method of claim 1, wherein: the pressure of the pressure forming is 9-11 MPa.
10. The method of claim 1, wherein: the drying temperature is 180-200 ℃.
11. The method of claim 1, wherein: the nitrogen pressure is more than or equal to 0.3 MPa.
12. The method of claim 1, wherein: the formed object is heated in a pushed slab kiln.
13. The method of claim 1, wherein: cooling to a temperature of less than or equal to 150 ℃, and discharging from the kiln.
14. The method of claim 13, wherein: and cooling to a temperature of less than or equal to 100 ℃, and discharging from the kiln.
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| CN109694982B (en) * | 2019-03-13 | 2020-06-30 | 湖北晶洋科技股份有限公司 | Preparation process of vanadium-nitrogen alloy |
| CN113621792A (en) * | 2021-08-05 | 2021-11-09 | 陕西中钒昌盛新材料科技有限公司 | Method for treating vanadium-nitrogen oxide alloy |
| 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 |
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