CN105803243A - Method for preparing vanadium-nitrogen alloy with inactive vanadium pentoxide catalyst - Google Patents
Method for preparing vanadium-nitrogen alloy with inactive vanadium pentoxide catalyst Download PDFInfo
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- CN105803243A CN105803243A CN201610173034.XA CN201610173034A CN105803243A CN 105803243 A CN105803243 A CN 105803243A CN 201610173034 A CN201610173034 A CN 201610173034A CN 105803243 A CN105803243 A CN 105803243A
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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Abstract
The invention relates to a method for preparing a vanadium-nitrogen alloy with an inactive vanadium pentoxide catalyst, and belongs to the technical field of alloy preparation. The method comprises the following steps: first, igniting a magnesium ribbon to release a large quantity of heat; carrying out a reaction between aluminum powder and ferriferous oxide to generate a large quantity of heat; carrying out a reaction between residual aluminum powder and inactive vanadium pentoxide under a high-temperature condition and protection of nitrogen to obtain a mixture of magnesium nitride, molten iron, aluminum oxide and the like; removing a mixture, floating on the surface of a molten iron mixture, of aluminum oxide and the like; and burning the left mixture to obtain the vanadium-nitrogen alloy. During preparation of the vanadium-nitrogen alloy, the reactions can be carried out according to internal temperatures, and deliberate temperature control is avoided, so that the operation is simple; and as the inactive vanadium pentoxide catalyst is taken as a main raw material, the resource is recovered and reused, and the cost is reduced.
Description
Technical field
The present invention relates to a kind of method utilizing inactivation vanadium pentoxide catalyst to prepare VN alloy, belong to field of alloy preparation technology.
Background technology
VN alloy is a kind of novel alloy additive, the vanadium iron production for micro alloyed steel can be substituted, vanadium nitride makes an addition to and can improve the comprehensive mechanical performances such as the intensity of steel, toughness, ductility and thermal fatigue resistance in steel, and make steel have good solderability, under reaching same intensity, add vanadium nitride and save vanadium addition 30-40%, and then reduce cost.In recent years, due to the obvious technology of V-n Microalloying Technology and economic advantages so that vanadium nitrogen microalloy is widely used in the development & production of the products such as high strength cast iron, non-hardened and tempered steel, high intensity strip, CSP product, high-strength plank and heavy wall H profile steel, seamless steel pipe, tool steel.Particularly in the popularization gradually of China, the development of VN alloy technology also achieves tangible result.
At present, the commercial run that VN alloy produces is varied, but divides direct material, mainly has two kinds of techniques: one adds carbonaceous reducing agent high temperature reduction Nitration synthesis VN alloy with vanadic anhydride；One adds carbonaceous reducing agent high temperature reduction Nitration synthesis VN alloy with Vanadium sesquioxide.Wherein the first technique is due to vanadic anhydride fusing point low (690 DEG C), to make it be completely reformed into the higher vanadium tetraoxide of fusing point or Vanadium sesquioxide before being changed into liquid phase in VN alloy production process, and temperature control requirement is harsh, and equipment requirements is high.The second technique, unstable under Vanadium sesquioxide normality, it is easily oxidized to high price vanadium in atmosphere, causes the storage difficulty of raw material, Vanadium sesquioxide purity is difficult to ensure that, causes production instability.
Summary of the invention
The technical problem to be solved: during for the current method producing VN alloy, harsh and raw material the storage of temperature control requirement is difficult; cause and produce unstable problem; provide a kind of first with the magnesium ribbon substantial amounts of heat of releasing lighted; make aluminium powder and ferroso-ferric oxide reaction; again release substantial amounts of heat; wherein react remaining aluminium powder again to react under hot conditions and nitrogen protection with inactivation vanadic anhydride; final removal aluminium sesquioxide mixture, then through the method that calcining can obtain VN alloy.The present invention, when preparing VN alloy, can react according to internal temperature, it is not necessary to deliberately controls temperature, and what utilize is the vanadium pentoxide catalyst of inactivation, and resource recycling saves cost.
For solving above-mentioned technical problem, the present invention adopts the technical scheme as described below to be:
(1) 120～150g vanadium pentoxide catalyst for inactivating after preparing sulphuric acid is weighed, after being rinsed well with clear water and naturally dried, it is placed in ball mill and carries out ball milling and cross 150 mesh sieves, obtain ball milling granule, being put in tube furnace by ball milling granule and calcine, controlling calcining heat is 150～170 DEG C, after calcining 45～55min, stand cooling, obtain pretreatment vanadium oxide particles；
(2) the pretreatment vanadium oxide particles of above-mentioned preparation is laid on crucible bottom, and above pretreatment vanadium oxide particles, it is sprinkled into 70～80g ferroferric oxide powder and mixture that 200～250g aluminium sesquioxide powder mixes, above mixture, then spread one layer of 0.5～0.7cm thickness magnesium powder again；
(3) after above-mentioned laying terminates, being inserted in magnesium powder by the magnesium ribbon of 7～8cm, light magnesium ribbon and be slowly introducing nitrogen simultaneously in crucible, it is 15～20mL/s that control nitrogen passes into speed, after passing into 40～55min so that it is continue reaction 1～2h；
(4) after question response terminates; after while hot the aluminium sesquioxide mixture floated on above crucible being removed; being placed in calcining furnace by remaining mixture in crucible, and calcine under nitrogen protection, calcining heat is 300～450 DEG C; calcination time is 50～55min; after calcining terminates, then it is cooled to 70～80 DEG C with the rate program of 2 DEG C/min, insulation reaction 30～40min; come out of the stove, VN alloy prepared by inactivation vanadium pentoxide catalyst can be obtained by.
Principles of the invention: release substantial amounts of heat first with the magnesium ribbon lighted; make aluminium powder and ferroso-ferric oxide reaction; again release substantial amounts of heat; wherein react remaining aluminium powder again to react under hot conditions and nitrogen protection with inactivation vanadic anhydride; obtain magnesium nitride; after the mixture such as molten iron and aluminium sesquioxide powder, then remove the aluminium sesquioxide mixture floating on molten iron mixture surface, finally remaining mixture calcining can be obtained VN alloy.
VN alloy vanadium content prepared by the present invention is 79～84%, and nitrogen content is 10～12%, and its density is 3.45～4.56g/cm3。
The present invention is compared with additive method, and Advantageous Effects is:
(1) when preparing VN alloy, can react according to internal temperature, it is not necessary to deliberately control temperature, simple to operate；
(2) VN alloy prepared by the present invention is mainly with the vanadium pentoxide catalyst of inactivation for raw material, and resource recycling saves cost.
Detailed description of the invention
First 120～the 150g vanadium pentoxide catalyst for inactivating after preparing sulphuric acid is weighed, after being rinsed well with clear water and naturally dried, it is placed in ball mill and carries out ball milling and cross 150 mesh sieves, obtain ball milling granule, being put in tube furnace by ball milling granule and calcine, controlling calcining heat is 150～170 DEG C, after calcining 45～55min, stand cooling, obtain pretreatment vanadium oxide particles；Again the pretreatment vanadium oxide particles of above-mentioned preparation is laid on crucible bottom, and above pretreatment vanadium oxide particles, it is sprinkled into 70～80g ferroferric oxide powder and mixture that 200～250g aluminium sesquioxide powder mixes, above mixture, then spread one layer of 0.5～0.7cm thickness magnesium powder again；After above-mentioned laying terminates, being inserted in magnesium powder by the magnesium ribbon of 7～8cm, light magnesium ribbon and be slowly introducing nitrogen simultaneously in crucible, it is 15～20mL/s that control nitrogen passes into speed, after passing into 40～55min so that it is continue reaction 1～2h；After question response terminates; after while hot the aluminium sesquioxide mixture floated on above crucible being removed; being placed in calcining furnace by remaining mixture in crucible, and calcine under nitrogen protection, calcining heat is 300～450 DEG C; calcination time is 50～55min; after calcining terminates, then it is cooled to 70～80 DEG C with the rate program of 2 DEG C/min, insulation reaction 30～40min; come out of the stove, VN alloy prepared by inactivation vanadium pentoxide catalyst can be obtained by.
Example 1
First the 150g vanadium pentoxide catalyst for inactivating after preparing sulphuric acid is weighed, after being rinsed well with clear water and naturally dried, it is placed in ball mill and carries out ball milling and cross 150 mesh sieves, obtain ball milling granule, being put in tube furnace by ball milling granule and calcine, controlling calcining heat is 170 DEG C, after calcining 55min, stand cooling, obtain pretreatment vanadium oxide particles；Again the pretreatment vanadium oxide particles of above-mentioned preparation is laid on crucible bottom, and above pretreatment vanadium oxide particles, it is sprinkled into 80g ferroferric oxide powder and mixture that 250g aluminium sesquioxide powder mixes, above mixture, then spread one layer of 0.7cm thickness magnesium powder again；After above-mentioned laying terminates, being inserted in magnesium powder by the magnesium ribbon of 8cm, light magnesium ribbon and be slowly introducing nitrogen simultaneously in crucible, it is 20mL/s that control nitrogen passes into speed, after passing into 55min so that it is continue reaction 2h；After question response terminates; after while hot the aluminium sesquioxide mixture floated on above crucible being removed; being placed in calcining furnace by remaining mixture in crucible, and calcine under nitrogen protection, calcining heat is 450 DEG C; calcination time is 55min; after calcining terminates, then it is cooled to 80 DEG C with the rate program of 2 DEG C/min, insulation reaction 40min; come out of the stove, VN alloy prepared by inactivation vanadium pentoxide catalyst can be obtained by.After testing, VN alloy vanadium content is 84%, and nitrogen content is 12%, and its density is 4.56g/cm3。
Example 2
First the 120g vanadium pentoxide catalyst for inactivating after preparing sulphuric acid is weighed, after being rinsed well with clear water and naturally dried, it is placed in ball mill and carries out ball milling and cross 150 mesh sieves, obtain ball milling granule, being put in tube furnace by ball milling granule and calcine, controlling calcining heat is 150 DEG C, after calcining 45min, stand cooling, obtain pretreatment vanadium oxide particles；Again the pretreatment vanadium oxide particles of above-mentioned preparation is laid on crucible bottom, and above pretreatment vanadium oxide particles, it is sprinkled into 70g ferroferric oxide powder and mixture that 200g aluminium sesquioxide powder mixes, above mixture, then spread one layer of 0.5cm thickness magnesium powder again；After above-mentioned laying terminates, being inserted in magnesium powder by the magnesium ribbon of 7cm, light magnesium ribbon and be slowly introducing nitrogen simultaneously in crucible, it is 15mL/s that control nitrogen passes into speed, after passing into 40min so that it is continue reaction 1h；After question response terminates; after while hot the aluminium sesquioxide mixture floated on above crucible being removed; being placed in calcining furnace by remaining mixture in crucible, and calcine under nitrogen protection, calcining heat is 300 DEG C; calcination time is 50min; after calcining terminates, then it is cooled to 70 DEG C with the rate program of 2 DEG C/min, insulation reaction 30min; come out of the stove, VN alloy prepared by inactivation vanadium pentoxide catalyst can be obtained by.After testing, VN alloy vanadium content is 79%, and nitrogen content is 10%, and its density is 3.45g/cm3。
Example 3
First the 125g vanadium pentoxide catalyst for inactivating after preparing sulphuric acid is weighed, after being rinsed well with clear water and naturally dried, it is placed in ball mill and carries out ball milling and cross 150 mesh sieves, obtain ball milling granule, being put in tube furnace by ball milling granule and calcine, controlling calcining heat is 160 DEG C, after calcining 50min, stand cooling, obtain pretreatment vanadium oxide particles；Again the pretreatment vanadium oxide particles of above-mentioned preparation is laid on crucible bottom, and above pretreatment vanadium oxide particles, it is sprinkled into 75g ferroferric oxide powder and mixture that 220g aluminium sesquioxide powder mixes, above mixture, then spread one layer of 0.55cm thickness magnesium powder again；After above-mentioned laying terminates, being inserted in magnesium powder by the magnesium ribbon of 7cm, light magnesium ribbon and be slowly introducing nitrogen simultaneously in crucible, it is 17mL/s that control nitrogen passes into speed, after passing into 50min so that it is continue reaction 1h；After question response terminates; after while hot the aluminium sesquioxide mixture floated on above crucible being removed; being placed in calcining furnace by remaining mixture in crucible, and calcine under nitrogen protection, calcining heat is 400 DEG C; calcination time is 52min; after calcining terminates, then it is cooled to 75 DEG C with the rate program of 2 DEG C/min, insulation reaction 35min; come out of the stove, VN alloy prepared by inactivation vanadium pentoxide catalyst can be obtained by.After testing, VN alloy vanadium content is 80%, and nitrogen content is 11%, and its density is 3.55g/cm3。
Claims (1)
1. one kind utilizes the method that inactivation vanadium pentoxide catalyst prepares VN alloy, it is characterised in that concrete preparation process is:
(1) 120～150g vanadium pentoxide catalyst for inactivating after preparing sulphuric acid is weighed, after being rinsed well with clear water and naturally dried, it is placed in ball mill and carries out ball milling and cross 150 mesh sieves, obtain ball milling granule, being put in tube furnace by ball milling granule and calcine, controlling calcining heat is 150～170 DEG C, after calcining 45～55min, stand cooling, obtain pretreatment vanadium oxide particles；
(2) the pretreatment vanadium oxide particles of above-mentioned preparation is laid on crucible bottom, and above pretreatment vanadium oxide particles, it is sprinkled into 70～80g ferroferric oxide powder and mixture that 200～250g aluminium sesquioxide powder mixes, above mixture, then spread one layer of 0.5～0.7cm thickness magnesium powder again；
(3) after above-mentioned laying terminates, being inserted in magnesium powder by the magnesium ribbon of 7～8cm, light magnesium ribbon and be slowly introducing nitrogen simultaneously in crucible, it is 15～20mL/s that control nitrogen passes into speed, after passing into 40～55min so that it is continue reaction 1～2h；
(4) after question response terminates; after while hot the aluminium sesquioxide mixture floated on above crucible being removed; being placed in calcining furnace by remaining mixture in crucible, and calcine under nitrogen protection, calcining heat is 300～450 DEG C; calcination time is 50～55min; after calcining terminates, then it is cooled to 70～80 DEG C with the rate program of 2 DEG C/min, insulation reaction 30～40min; come out of the stove, VN alloy prepared by inactivation vanadium pentoxide catalyst can be obtained by.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106399786A (en) * | 2016-11-25 | 2017-02-15 | 南通汉瑞新材料科技有限公司 | Novel method for preparing vanadium-nitrogen alloy |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106399786A (en) * | 2016-11-25 | 2017-02-15 | 南通汉瑞新材料科技有限公司 | Novel method for preparing vanadium-nitrogen alloy |
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