Method for producing vanadium-nitrogen alloy with preset sulfur content
阅读说明：本技术 一种生产预定硫含量的钒氮合金的方法 (Method for producing vanadium-nitrogen alloy with preset sulfur content ) 是由 高雷章 师启华 陈海军 尹丹凤 于 2021-08-05 设计创作，主要内容包括：本发明涉及钒冶金技术领域,公开了一种生产预定硫含量的钒氮合金的方法。所述方法包括：(1)检测钒氧化物的硫含量W-(钒氧化物)；(2)将钒氧化物的硫含量W-(钒氧化物)和钒氮合金产品的预定硫含量W-(钒氮合金)代入公式中计算得到煅烧温度T,T的范围为1200-1800,单位为℃；(3)将钒氧化物和碳粉进行混合,得到混合料；(4)向步骤(3)得到的混合料中加水继续混合,然后成型,得到成型物料；(5)将步骤(4)得到的成型物料转移至煅烧装置中,然后在氮气气氛中并按照步骤(2)中计算得到的煅烧温度T进行煅烧,得到钒氮合金产品。本发明所述的方法可以实现对钒氮合金中杂质硫的含量的精准控制。(The invention relates to the technical field of vanadium metallurgy, and discloses a method for producing a vanadium-nitrogen alloy with preset sulfur content. The method comprises the following steps: (1) detecting the sulfur content W of vanadium oxide Vanadium oxide (ii) a (2) Sulfur content W of vanadium oxide Vanadium oxide And predetermined sulfur content W of the vanadium-nitrogen alloy product Vanadium-nitrogen alloy The calcination temperature T is calculated by substituting into a formula, the range of T is 1200-1800 and the unit is; (3) mixing vanadium oxide and carbon powder to obtain a mixture; (4) adding water into the mixture obtained in the step (3), continuously mixing, and then forming to obtain a formed material; (5) transferring the formed material obtained in the step (4) to a calcining device, and then calculating according to the step (2) in a nitrogen atmosphereAnd calcining at the obtained calcining temperature T to obtain the vanadium-nitrogen alloy product. The method can realize the accurate control of the content of the impurity sulfur in the vanadium-nitrogen alloy.)
1. A method of producing a vanadium-nitrogen alloy of a predetermined sulfur content, characterized in that it comprises the steps of:
(1) detecting the sulfur content W of vanadium oxideVanadium oxide；
(2) Sulfur content W of vanadium oxideVanadium oxideAnd predetermined sulfur content W of the vanadium-nitrogen alloy productVanadium-nitrogen alloyThe calcination temperature T is calculated by substituting the following formula (1), the range of T is 1200-1800 in unit,
wherein, WVanadium oxideAnd WVanadium-nitrogen alloyAre all weight percentages;
(3) mixing vanadium oxide and carbon powder to obtain a mixture;
(4) adding water into the mixture obtained in the step (3), continuously mixing, and then forming to obtain a formed material;
(5) and (3) transferring the formed material obtained in the step (4) to a calcining device, and calcining in a nitrogen atmosphere according to the calcining temperature T obtained in the step (2) to obtain a vanadium-nitrogen alloy product.
2. The method for producing a vanadium-nitrogen alloy with a predetermined sulfur content according to claim 1, wherein in the step (1), the vanadium oxide is vanadium oxide produced by reducing vanadium slag in steel making.
3. The method for producing a vanadium-nitrogen alloy of a predetermined sulfur content according to claim 1 or 2, characterized in that in step (3), the vanadium oxide contains 59 to 63% by weight of V, < 0.5% by weight of S, < 0.68% by weight of C, < 0.3% by weight of Na, < 0.13% by weight of P, and the balance of O.
4. The method for producing vanadium-nitrogen alloy with predetermined sulfur content according to claim 1 or 2, wherein in step (3), the carbon powder contains 98 wt% or more of C and 0.13 wt% or less of S.
5. The method for producing vanadium-nitrogen alloy with predetermined sulfur content in claim 1, wherein in the step (3), the weight ratio of the vanadium oxide to the carbon powder is 100 (24-26).
6. The method for producing vanadium-nitrogen alloy with predetermined sulfur content according to claim 1, wherein in the step (4), the amount of water is 2-4 wt% of the weight of the mixed material.
7. The method for producing vanadium-nitrogen alloy with predetermined sulfur content according to claim 1, wherein in the step (4), the forming mode is extrusion forming.
8. The method for producing a vanadium-nitrogen alloy with a predetermined sulfur content according to claim 1, wherein in the step (5), the purity of the nitrogen gas is 99.99%.
9. The method for producing vanadium-nitrogen alloy with predetermined sulfur content according to claim 1, wherein in the step (5), the calcining device is a pushed slab kiln, a rotary kiln or a vertical intermediate frequency furnace.
10. The method for producing vanadium-nitrogen alloy with predetermined sulfur content according to claim 1, wherein in the step (5), the calcination time is not less than 3 h.
Technical Field
The invention relates to the technical field of vanadium metallurgy, in particular to a method for producing a vanadium-nitrogen alloy with preset sulfur content.
Background
The vanadium-nitrogen alloy is a compound generated by vanadium and nitrogen, and is a novel alloy additive. The industrial production adopts vanadium oxide, carbon and nitrogen to react and synthesize. The vanadium-nitrogen alloy can replace ferrovanadium to be used for producing microalloyed steel, and can improve the comprehensive mechanical properties of the steel, such as strength, toughness, ductility, thermal fatigue resistance and the like when being added into the steel, and the steel has good weldability. Under the condition of achieving the same strength, the vanadium-nitrogen alloy is added, so that the adding amount of vanadium is saved by 30-40%, and the cost is further reduced.
However, the promotion of the steel performance is reduced due to the excessively high content of S in the vanadium-nitrogen alloy, the steel performance is improved to the same level by using the low-sulfur vanadium-nitrogen alloy and the high-sulfur vanadium-nitrogen alloy, more high-sulfur vanadium-nitrogen alloy is required to be added, and the subsequent use of the steel is greatly influenced. Therefore, it is necessary to control the sulfur content in the vanadium-nitrogen alloy. The content of S is regulated to be less than or equal to 0.1 percent in the national standard GB/T20567-2020 of vanadium-nitrogen alloy
Therefore, how to produce vanadium-nitrogen alloy with controllable impurity sulfur content is one of the problems to be solved urgently by researchers in the field.
Disclosure of Invention
The invention aims to solve the problems that the sulfur content of raw material vanadium oxide is higher and the calcination result of the sulfur content is difficult to control in the production process of vanadium-nitrogen alloy in the prior art, and provides a method for producing vanadium-nitrogen alloy with preset sulfur content.
In order to achieve the above object, the present invention provides a method of producing a vanadium-nitrogen alloy of a predetermined sulfur content, the method comprising the steps of:
(1) detecting the sulfur content W of vanadium oxideVanadium oxide；
(2) Sulfur content W of vanadium oxideVanadium oxideAnd predetermined sulfur content W of the vanadium-nitrogen alloy productVanadium-nitrogen alloyThe calcination temperature T is calculated by substituting the following formula (1), the range of T is 1200-1800 in unit,
wherein, WVanadium oxideAnd WVanadium-nitrogen alloyAre all weight percentages;
(3) mixing vanadium oxide and carbon powder to obtain a mixture;
(4) adding water into the mixture obtained in the step (3), continuously mixing, and then forming to obtain a formed material;
(5) and (3) transferring the formed material obtained in the step (4) to a calcining device, and calcining in a nitrogen atmosphere according to the calcining temperature T obtained in the step (2) to obtain a vanadium-nitrogen alloy product.
Preferably, in the step (3), the vanadium oxide is vanadium oxide produced by reduction of steelmaking vanadium slag.
Preferably, in step (3), the vanadium oxide contains 59 to 63 wt% of V, <0.5 wt% of S, < 0.68 wt% of C, < 0.3 wt% of Na, < 0.13 wt% of P, and the balance of O.
Preferably, in step (3), the carbon powder contains more than or equal to 98 weight percent of C and less than or equal to 0.13 weight percent of S.
Preferably, in the step (3), the weight ratio of the vanadium oxide to the carbon powder is 100 (24-26).
Preferably, in step (4), the amount of water is 2-4 wt% of the weight of the mix.
Preferably, in the step (4), the forming mode is extrusion forming.
Preferably, in step (5), the nitrogen has a purity of 99.99%.
Preferably, in the step (5), the calcining device is a pushed slab kiln, a rotary kiln or a vertical intermediate frequency furnace.
Preferably, in step (5), the calcination time is not less than 3 h.
In the invention, in the preparation process of the vanadium-nitrogen alloy, the optimal calcination temperature in the range of 1200-1800 ℃ can be calculated through the preset sulfur content in the vanadium-nitrogen alloy and the sulfur content of the raw material vanadium oxide, and then the vanadium-nitrogen alloy with the preset sulfur content can be prepared by calcining at the optimal calcination temperature. The method can realize the accurate control of the content of the impurity sulfur in the vanadium-nitrogen alloy.
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The inventors of the present invention found in the course of research that, in the preparation of vanadium-nitrogen alloy, when the calcination temperature is in the range of 1200-1800 ℃, the sulfur content in the raw material vanadium oxide, the calcination temperature and the sulfur content in the vanadium-nitrogen alloy satisfy the formula (1), based on which the present invention was accomplished.
The invention provides a method for producing vanadium-nitrogen alloy with preset sulfur content, which comprises the following steps:
(1) detecting the sulfur content W of vanadium oxideVanadium oxide；
(2) Sulfur content W of vanadium oxideVanadium oxideAnd predetermined sulfur content W of the vanadium-nitrogen alloy productVanadium-nitrogen alloyThe calcination temperature T is calculated by substituting the following formula (1), the range of T is 1200-1800 in unit,
wherein, WVanadium oxideAnd WVanadium-nitrogen alloyAre all weight percentages;
(3) mixing vanadium oxide and carbon powder to obtain a mixture;
(4) adding water into the mixture obtained in the step (3), continuously mixing, and then forming to obtain a formed material;
(5) and (3) transferring the formed material obtained in the step (4) to a calcining device, and calcining in a nitrogen atmosphere according to the calcining temperature T obtained in the step (2) to obtain a vanadium-nitrogen alloy product.
In a preferred embodiment, in step (3), the vanadium oxide is steelmaking vanadium oxide.
Further preferably, in step (3), the vanadium oxide contains 59 to 63 wt% of V, <0.5 wt% of S, < 0.68 wt% of C, < 0.3 wt% of Na, < 0.13 wt% of P, and the balance of O.
Even more preferably, the vanadium oxide contains < 0.3 wt.% S.
In a preferred embodiment, in step (3), the carbon powder contains 98 wt% or more of C and 0.13 wt% or less of S.
In a preferred embodiment, in the step (3), the weight ratio of the vanadium oxide to the carbon powder is 100 (24-26).
In a preferred embodiment, in step (4), the water is used in an amount of 2 to 4% by weight based on the weight of the mix.
In a preferred embodiment, in the step (4), the molding is extrusion molding.
In a preferred embodiment, in the step (4), the shape of the molding material may be a sphere.
Preferably, in step (5), the nitrogen has a purity of 99.99%.
Preferably, in the step (5), the calcining device is a pushed slab kiln, a rotary kiln or a vertical intermediate frequency furnace. Further preferably, the calcining device is a pushed slab kiln.
Preferably, in step (5), the calcination time is 3h or more. Further preferably, the calcining time is 3-5 h.
In a specific embodiment, an optimum calcination temperature can be obtained according to the formula (1) for the range of the sulfur content of impurities required by actual production, such as the limited range of the sulfur content in vanadium-nitrogen alloy in national standard GB/T20567-.
The present invention will be described in detail below by way of examples, but the scope of the present invention is not limited thereto.
The carbon powder used in the following examples contained 98 wt% of C and 0.13 wt% of S.
Example 1
The method for producing the vanadium-nitrogen alloy with the preset sulfur content of 0.1287 percent comprises the following steps:
(1) detecting the sulfur content W of vanadium oxideVanadium oxideResult is WVanadium oxide0.15 wt%, other elements content: 62.3 wt% V, 0.08 wt% C, 0.3 wt% Na, 0.1 wt% P, and the balance O.
(2) Sulfur content W of vanadium oxideVanadium oxideAnd predetermined sulfur content W of the vanadium-nitrogen alloy productVanadium-nitrogen alloyThe calcination temperature T is calculated by substituting the following formula (1), the range of T is 1200-1800 in unit,
wherein, WVanadium oxideAnd WVanadium-nitrogen alloyAre all weight percentages;
the result is T1400;
(3) mixing vanadium oxide and carbon powder according to the weight ratio of 100:25 to obtain a mixture;
(4) adding water (the amount is 4% of the weight of the mixture) into the mixture obtained in the step (3), continuously mixing, and then carrying out extrusion forming to obtain a formed material;
(5) and (3) transferring the formed material obtained in the step (4) to a pushed slab kiln, and then calcining in a nitrogen (with the purity of 99.99%) atmosphere at the temperature obtained by calculation in the step (2) for 6 hours to obtain the vanadium-nitrogen alloy.
In this embodiment, the actual value W of the sulfur content in the obtained vanadium-nitrogen alloy is detectedVanadium-nitrogen alloy0.13% by weight.
Example 2
The method for producing the vanadium-nitrogen alloy with the preset sulfur content of 0.1161 percent comprises the following steps:
(1) detecting the sulfur content W of vanadium oxideVanadium oxideResult is WVanadium oxide0.15 wt%, other elements content: 62.3 wt% V, 0.08 wt% C, 0.3 wt% Na, 0.1 wt% P, and the balance O.
(2) Sulfur content W of vanadium oxideVanadium oxideAnd predetermined sulfur content W of the vanadium-nitrogen alloy productVanadium-nitrogen alloyThe calcination temperature T is calculated by substituting the following formula (1), the range of T is 1200-1800 in unit,
wherein, WVanadium oxideAnd WVanadium-nitrogen alloyAre all weight percentages;
the result is T1450;
(3) mixing vanadium oxide and carbon powder according to the weight ratio of 100:25 to obtain a mixture;
(4) adding water (the amount is 4% of the weight of the mixture) into the mixture obtained in the step (3), continuously mixing, and then carrying out extrusion forming to obtain a formed material;
(5) and (3) transferring the formed material obtained in the step (4) to a pushed slab kiln, and then calcining in a nitrogen (with the purity of 99.99%) atmosphere at the temperature obtained by calculation in the step (2) for 5 hours to obtain the vanadium-nitrogen alloy.
In this embodimentIn the detected actual value W of the sulfur content in the obtained vanadium-nitrogen alloyVanadium-nitrogen alloy0.12% by weight.
Example 3
The vanadium-nitrogen alloy with the preset sulfur content of 0.099% is produced, and the specific preparation process comprises the following steps:
(1) detecting the sulfur content W of vanadium oxideVanadium oxideResult is WVanadium oxide0.15 wt%, other elements content: 62.3 wt% V, 0.08 wt% C, 0.3 wt% Na, 0.1 wt% P, and the balance O.
(2) Sulfur content W of vanadium oxideVanadium oxideAnd predetermined sulfur content W of the vanadium-nitrogen alloy productVanadium-nitrogen alloyThe calcination temperature T is calculated by substituting the following formula (1), the range of T is 1200-1800 in unit,
wherein, WVanadium oxideAnd WVanadium-nitrogen alloyAre all weight percentages;
the result is T1500;
(3) mixing vanadium oxide and carbon powder according to the weight ratio of 100:25 to obtain a mixture;
(4) adding water (the amount is 4% of the weight of the mixture) into the mixture obtained in the step (3), continuously mixing, and then carrying out extrusion forming to obtain a formed material;
(5) and (3) transferring the formed material obtained in the step (4) to a pushed slab kiln, and then calcining in a nitrogen (with the purity of 99.99%) atmosphere at the temperature obtained by calculation in the step (2) for 4 hours to obtain the vanadium-nitrogen alloy.
In this embodiment, the actual value W of the sulfur content in the obtained vanadium-nitrogen alloy is detectedVanadium-nitrogen alloy0.10% by weight.
Example 4
The method for producing the vanadium-nitrogen alloy with the preset sulfur content of 0.083% comprises the following steps:
(1) detecting the sulfur content W of vanadium oxideVanadium oxideResult is WVanadium oxide0.16 wt%, and the contents of other elements are: 62.0 wt% V, 0.11 wt% C, 0.27 wt% Na, 0.11 wt% P, and the balance O.
(2) Sulfur content W of vanadium oxideVanadium oxideAnd predetermined sulfur content W of the vanadium-nitrogen alloy productVanadium-nitrogen alloyThe calcination temperature T is calculated by substituting the following formula (1), the range of T is 1200-1800 in unit,
wherein, WVanadium oxideAnd WVanadium-nitrogen alloyAre all weight percentages;
the result is T1550;
(3) mixing vanadium oxide and carbon powder according to the weight ratio of 100:25 to obtain a mixture;
(4) adding water (the amount is 4% of the weight of the mixture) into the mixture obtained in the step (3), continuously mixing, and then carrying out extrusion forming to obtain a formed material;
(5) and (3) transferring the formed material obtained in the step (4) to a pushed slab kiln, and then calcining in a nitrogen (with the purity of 99.99%) atmosphere at the temperature obtained by calculation in the step (2) for 4 hours to obtain the vanadium-nitrogen alloy.
In this embodiment, the actual value W of the sulfur content in the obtained vanadium-nitrogen alloy is detectedVanadium-nitrogen alloy0.07 wt.%.
Example 5
The method for producing the vanadium-nitrogen alloy with the preset sulfur content of 0.0943 percent comprises the following steps:
(1) detecting the sulfur content W of vanadium oxideVanadium oxideResult is WVanadium oxide0.18 wt%, V with a content of other elements of 61.2 wt%, 0.37 wt% C, 0.28 wt% Na, 0.13 wt% P, and the balance O.
(2) Will be provided withSulfur content W of vanadium oxideVanadium oxideAnd predetermined sulfur content W of the vanadium-nitrogen alloy productVanadium-nitrogen alloyThe calcination temperature T is calculated by substituting the following formula (1), the range of T is 1200-1800 in unit,
wherein, WVanadium oxideAnd WVanadium-nitrogen alloyAre all weight percentages;
the result is T1550;
(3) mixing vanadium oxide and carbon powder according to the weight ratio of 100:25 to obtain a mixture;
(4) adding water (the amount is 4% of the weight of the mixture) into the mixture obtained in the step (3), continuously mixing, and then carrying out extrusion forming to obtain a formed material;
(5) and (3) transferring the formed material obtained in the step (4) to a pushed slab kiln, and then calcining in a nitrogen (with the purity of 99.99%) atmosphere at the temperature obtained by calculation in the step (2) for 4 hours to obtain the vanadium-nitrogen alloy.
In this embodiment, the actual value W of the sulfur content in the obtained vanadium-nitrogen alloy is detectedVanadium-nitrogen alloy0.08% by weight. .
Example 6
The method for producing the vanadium-nitrogen alloy with the preset sulfur content of 0.0845 percent comprises the following steps:
(1) detecting the sulfur content W of vanadium oxideVanadium oxideResult is WVanadium oxide0.22 wt%, V with a content of other elements of 60.9 wt%, 0.68 wt% C, 0.26 wt% Na, 0.09 wt% P, and the balance O.
(2) Sulfur content W of vanadium oxideVanadium oxideAnd predetermined sulfur content W of the vanadium-nitrogen alloy productVanadium-nitrogen alloyThe calcination temperature T is calculated by substituting the following formula (1), the range of T is 1200-1800 in unit,
wherein, WVanadium oxideAnd WVanadium-nitrogen alloyAre all weight percentages;
the result is T1600;
(3) mixing vanadium oxide and carbon powder according to the weight ratio of 100:25 to obtain a mixture;
(4) adding water (the amount is 4% of the weight of the mixture) into the mixture obtained in the step (3), continuously mixing, and then carrying out extrusion forming to obtain a formed material;
(5) and (3) transferring the formed material obtained in the step (4) to a pushed slab kiln, and then calcining in a nitrogen (with the purity of 99.99%) atmosphere at the temperature obtained by calculation in the step (2) for 4 hours to obtain the vanadium-nitrogen alloy.
In this embodiment, the actual value W of the sulfur content in the obtained vanadium-nitrogen alloy is detectedVanadium-nitrogen alloy0.06 wt%. .
Test example
The deviation between the expected value and the measured value of the sulfur content in the vanadium-nitrogen alloy described in the examples was calculated, and the results are shown in table 1.
TABLE 1 comparison of expected values with measured values
As can be seen from table 1, the sulfur content in the vanadium-nitrogen alloy prepared by the method of the present invention has a smaller deviation than the expected value, which indicates that the sulfur content in the vanadium-nitrogen alloy can be controlled by the method of the present invention, and the vanadium-nitrogen alloy meeting the predetermined value can be prepared. In this case, when the temperature is 1550 ℃ or higher, the difference between the expected value and the actually measured value is slightly large, because the amount of S accompanying the increase of the temperature is increased outside the system.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
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