CN106498266B - A kind of preparation method of VN alloy - Google Patents
A kind of preparation method of VN alloy Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229910045601 alloy Inorganic materials 0.000 title description 2
- 239000000956 alloy Substances 0.000 title description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 51
- SKKMWRVAJNPLFY-UHFFFAOYSA-N azanylidynevanadium Chemical compound [V]#N SKKMWRVAJNPLFY-UHFFFAOYSA-N 0.000 claims abstract description 38
- 229910001199 N alloy Inorganic materials 0.000 claims abstract description 37
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 27
- 239000000463 material Substances 0.000 claims abstract description 27
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 25
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 22
- UUUGYDOQQLOJQA-UHFFFAOYSA-L vanadyl sulfate Chemical compound [V+2]=O.[O-]S([O-])(=O)=O UUUGYDOQQLOJQA-UHFFFAOYSA-L 0.000 claims abstract description 18
- 229940041260 vanadyl sulfate Drugs 0.000 claims abstract description 18
- 229910000352 vanadyl sulfate Inorganic materials 0.000 claims abstract description 18
- 239000002245 particle Substances 0.000 claims abstract description 12
- 239000006229 carbon black Substances 0.000 claims abstract description 7
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 7
- 239000010439 graphite Substances 0.000 claims abstract description 7
- 239000013590 bulk material Substances 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 abstract description 14
- 238000006243 chemical reaction Methods 0.000 abstract description 8
- 230000035484 reaction time Effects 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract description 2
- 238000003825 pressing Methods 0.000 abstract description 2
- 229910052720 vanadium Inorganic materials 0.000 description 14
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 14
- 229910000831 Steel Inorganic materials 0.000 description 7
- 239000010959 steel Substances 0.000 description 7
- 239000011230 binding agent Substances 0.000 description 6
- 238000005121 nitriding Methods 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 description 2
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 229910001935 vanadium oxide Inorganic materials 0.000 description 2
- 229910000640 Fe alloy Inorganic materials 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 229910000756 V alloy Inorganic materials 0.000 description 1
- QUEDYRXQWSDKKG-UHFFFAOYSA-M [O-2].[O-2].[V+5].[OH-] Chemical compound [O-2].[O-2].[V+5].[OH-] QUEDYRXQWSDKKG-UHFFFAOYSA-M 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000010903 husk Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- PNXOJQQRXBVKEX-UHFFFAOYSA-N iron vanadium Chemical compound [V].[Fe] PNXOJQQRXBVKEX-UHFFFAOYSA-N 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C35/00—Master alloys for iron or steel
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/02—Alloys based on vanadium, niobium, or tantalum
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
本发明涉及一种钒氮合金的制备方法。其技术方案是：将碳质还原剂和以无水物计的硫酸氧钒按质量比为(0.1~0.3)∶1配料，混匀，得到混合物料。将所述混合物料机压为块状物料，所述块状物料的密度为1.5~2.0g/cm3；再将所述块状物料在60~120℃条件下干燥1~7h。在常压和氮气流量为100~600mL/min的条件下，将干燥后的块状物料加热至1000~1400℃，保温1~5h，随炉冷却至室温~100℃，出炉，得到钒氮合金。所述碳质还原剂为碳黑、石墨和活性炭中的一种以上，所述碳质还原剂的粒度为0.074~0.250mm；所述硫酸氧钒的粒度为0.074~0.250mm。本发明具有工艺简单、反应时间短和反应温度低的特点。The invention relates to a preparation method of vanadium nitrogen alloy. The technical scheme is as follows: the carbonaceous reducing agent and vanadyl sulfate calculated as anhydrous matter are mixed according to the mass ratio of (0.1-0.3): 1, and mixed to obtain a mixed material. Pressing the mixed material into a block material with a density of 1.5-2.0 g/cm 3 ; then drying the block material at 60-120° C. for 1-7 hours. Under the conditions of normal pressure and nitrogen flow rate of 100~600mL/min, heat the dried bulk material to 1000~1400°C, keep it warm for 1~5h, cool to room temperature~100°C with the furnace, and take it out of the furnace to obtain vanadium nitrogen alloy . The carbonaceous reducing agent is more than one of carbon black, graphite and activated carbon, the particle size of the carbonaceous reducing agent is 0.074-0.250mm; the particle size of the vanadyl sulfate is 0.074-0.250mm. The invention has the characteristics of simple process, short reaction time and low reaction temperature.
Description
技术领域technical field
本发明属于钒合金技术领域。具体涉及一种钒氮合金的制备方法。The invention belongs to the technical field of vanadium alloys. Specifically relates to a preparation method of vanadium nitrogen alloy.
背景技术Background technique
钒氮合金是一种新型的合金添加剂，添加于钢中能够通过析出强化和细晶强化提高钢的强度、韧性、延展性、耐磨性、耐腐蚀性和抗热疲劳性等综合机械性能，能够有效改善钢的焊接性能。与钢中添加钒铁合金相比，在相同的强度下可以节约钒量20~40%，从而降低了钢铁合金化成本。含钒钢中氮含量从40ppm上升到160ppm时，屈服强度增大了110MPa，因此，提高钒氮合金中的氮含量，能有效节约钢材用量，即能节约原料和冶炼成本，具有巨大的资源节约和环境保护的双重效益。Vanadium-nitrogen alloy is a new type of alloy additive. Adding it to steel can improve the comprehensive mechanical properties of steel such as strength, toughness, ductility, wear resistance, corrosion resistance and thermal fatigue resistance through precipitation strengthening and fine grain strengthening. It can effectively improve the welding performance of steel. Compared with adding vanadium-iron alloy to steel, the amount of vanadium can be saved by 20-40% under the same strength, thus reducing the cost of steel alloying. When the nitrogen content in the vanadium-containing steel increases from 40ppm to 160ppm, the yield strength increases by 110MPa. Therefore, increasing the nitrogen content in the vanadium-nitrogen alloy can effectively save the amount of steel, that is, it can save raw materials and smelting costs, and has a huge resource saving and environmental protection dual benefits.
传统的钒氮合金的制备方法是将五氧化二钒、四氧化二钒、三氧化二钒、偏钒酸铵、多钒酸铵等作为原料，配加还原剂、粘结剂、促进剂等，在高温下与氮气或氨气反应生成钒氮合金产品。The traditional preparation method of vanadium nitrogen alloy is to use vanadium pentoxide, vanadium tetroxide, vanadium trioxide, ammonium metavanadate, ammonium polyvanadate, etc. as raw materials, and add reducing agent, binder, accelerator, etc. , react with nitrogen or ammonia at high temperature to produce vanadium nitrogen alloy products.
“一种简易氮化钒的生产方法”（CN102173395A）专利技术，以V2O5和石墨粉为原料，混匀后加入粘结剂聚乙烯醇水溶液，湿混后压球，干燥，在800℃预还原5h左右，升温至1350℃持续大于6h的深度还原和碳化，在此过程中不断充入99.99%以上的氮气；继续升温至1600℃，进行6~10h的氮化烧结，此过程压力为0.02MPa，总时间在20h左右，反应完成，冷却至150℃出炉，制得钒氮合金。"A Simple Production Method of Vanadium Nitride" (CN102173395A) patented technology, using V 2 O 5 and graphite powder as raw materials, adding binder polyvinyl alcohol aqueous solution after mixing, pressing balls after wet mixing, drying, at 800 Pre-reduction at ℃ for about 5 hours, the temperature was raised to 1350 ℃, and the deep reduction and carbonization continued for more than 6 hours. During this process, more than 99.99% nitrogen was continuously filled; 0.02MPa, the total time is about 20h, the reaction is completed, cooled to 150 ℃ out of the furnace, and the vanadium nitrogen alloy is obtained.
“一种制备钒氮合金的方法”（CN103952512A）专利技术，由偏钒酸铵或/和多钒酸铵在氮氢混合气氛下于600~650℃还原3~6h，得到钒氧化物；将得到的钒氧化物与催化剂、碳质粉剂、粘结剂和水湿法制球，在常压氮气氛下于300~350℃保温1~3h，然后升温至1450~1650℃，充入压力为正0.04~0.08MPa的氮气，进行氮化反应6~9h，降温出料，获得钒氮合金。"A method for preparing vanadium-nitrogen alloy" (CN103952512A) patented technology, by reducing ammonium metavanadate or/and ammonium polyvanadate at 600-650°C for 3-6 hours in a nitrogen-hydrogen mixed atmosphere to obtain vanadium oxide; The obtained vanadium oxide, catalyst, carbonaceous powder, binder and water-wet method balls are kept at 300-350°C for 1-3h under normal pressure nitrogen atmosphere, then the temperature is raised to 1450-1650°C, and the filling pressure is positive. 0.04~0.08MPa nitrogen gas, carry out nitriding reaction for 6~9h, cool down and discharge, and obtain vanadium nitrogen alloy.
“一种钒氮合金生产方法”（CN102936678A）专利技术，将含钒原料粉、铁粉、碳质粉剂和粘结剂搅拌混合后压块成型，再与稻壳按体积比1∶1的比例送入煅烧窑，无氧条件下干馏处理，温度为600~650℃，时间为6~7h，然后加热到1300~1500℃，同时通入高纯氮气，时间2~4h，冷却出炉获得氮化钒产品。"A production method of vanadium-nitrogen alloy" (CN102936678A) patented technology, mixing vanadium-containing raw material powder, iron powder, carbonaceous powder and binder, then briquetting, and then mixing with rice husk in a volume ratio of 1:1 Send it to the calcination kiln, dry distillation treatment under anaerobic conditions, the temperature is 600~650°C, the time is 6~7h, and then heated to 1300~1500°C, and high-purity nitrogen is introduced at the same time, the time is 2~4h, and the furnace is cooled to obtain nitriding Vanadium products.
上述生产方法制备的钒氮合金中氮含量较高，但存在的缺点是：工艺复杂、生产周期长和制备温度高。The vanadium-nitrogen alloy prepared by the above production method has relatively high nitrogen content, but has the disadvantages of complex process, long production cycle and high preparation temperature.
发明内容Contents of the invention
本发明旨在克服现有技术缺陷，目的是提供一种工艺简单、反应时间短和反应温度低的钒氮合金的制备方法。The invention aims to overcome the defects of the prior art, and aims to provide a method for preparing a vanadium-nitrogen alloy with simple process, short reaction time and low reaction temperature.
为实现上述目的，本发明采用的技术方案的具体步骤是：In order to achieve the above object, the concrete steps of the technical solution adopted in the present invention are:
步骤一、将碳质还原剂和以无水物计的硫酸氧钒按质量比为(0.1~0.3)∶1配料，混匀，得到混合物料。Step 1: The carbonaceous reducing agent and vanadyl sulfate calculated as anhydrous matter are mixed according to the mass ratio of (0.1-0.3): 1, and mixed to obtain a mixed material.
步骤二、将所述混合物料机压为块状物料，所述块状物料的密度为1.5~2.0g/cm3；再将所述块状物料在60~120℃条件下干燥1~7h。Step 2: press the mixed material into a block material with a density of 1.5-2.0 g/cm 3 ; then dry the block material at 60-120° C. for 1-7 hours.
步骤三、在常压和氮气流量为100~600mL/min的条件下，将干燥后的块状物料加热至1000~1400℃，保温1~5h，随炉冷却至室温~100℃，出炉，得到钒氮合金。Step 3. Under the conditions of normal pressure and nitrogen flow rate of 100-600mL/min, heat the dried bulk material to 1000-1400°C, keep it warm for 1-5h, cool it to room temperature-100°C with the furnace, and take it out of the furnace to obtain Vanadium nitrogen alloy.
所述碳质还原剂为碳黑、石墨和活性炭中的一种以上。The carbonaceous reducing agent is more than one of carbon black, graphite and activated carbon.
所述碳质还原剂的粒度为0.074~0.250mm。The particle size of the carbonaceous reducing agent is 0.074-0.250mm.
所述硫酸氧钒的粒度为0.074~0.250mm。The particle size of the vanadyl sulfate is 0.074-0.250mm.
由于采用上述技术方案，本发明的有益效果是：Owing to adopting above-mentioned technical scheme, the beneficial effect of the present invention is:
(1)本发明采用硫酸氧钒作为原料，由于硫酸氧钒含有结晶水和吸附水，在造块过程中无需外加粘结剂，工艺简单。(1) The present invention adopts vanadyl sulfate as raw material, because vanadyl sulfate contains crystallization water and adsorption water, does not need to add binder in the process of agglomeration, and process is simple.
(2)本发明采用的硫酸氧钒在加热过程中分解，使得物料的比表面积增大，增加了与氮气的接触面积，提高了还原氮化速率，增加了氮含量，无需外加促进剂且还原氮化时间短。(2) The vanadyl sulfate adopted in the present invention decomposes in the heating process, so that the specific surface area of the material is increased, the contact area with nitrogen is increased, the reduction nitriding rate is improved, the nitrogen content is increased, no additional accelerator is required and the reduction Nitriding time is short.
(3)本发明反应温度低，有利于节约能耗。(3) The reaction temperature of the present invention is low, which is beneficial to saving energy consumption.
本发明制备的钒氮合金经检测：钒含量为77.52~80.43wt%；氮含量为12.67~16.98wt%；表观密度为3.03~3.54g/cm3。The vanadium-nitrogen alloy prepared by the invention is tested: the vanadium content is 77.52-80.43wt%, the nitrogen content is 12.67-16.98wt%, and the apparent density is 3.03-3.54g/cm 3 .
因此，本发明具有工艺简单、反应时间短和反应温度低的特点。Therefore, the present invention has the characteristics of simple process, short reaction time and low reaction temperature.
具体实施方式Detailed ways
下面结合实施例对本发明技术方案做进一步详细的说明，并不将本发明限制在所述的实施例中。The technical solutions of the present invention will be further described in detail below in conjunction with the examples, and the present invention is not limited to the examples.
实施例1Example 1
一种钒氮合金的制备方法。本实施例采用的技术方案的具体步骤是：A preparation method of a vanadium nitrogen alloy. The concrete steps of the technical solution adopted in this embodiment are:
步骤一、将碳质还原剂和以无水物计的硫酸氧钒按质量比为(0.1~0.2)∶1配料，混匀，得到混合物料。Step 1. The carbonaceous reducing agent and the vanadyl sulfate calculated as anhydrous matter are mixed according to the mass ratio of (0.1-0.2): 1, and mixed to obtain a mixed material.
步骤二、将所述混合物料机压为块状物料，所述块状物料的密度为1.5~1.8g/cm3；再将所述块状物料在60~120℃条件下干燥1~7h。Step 2: press the mixed material into a block material with a density of 1.5-1.8 g/cm 3 ; and then dry the block material at 60-120° C. for 1-7 hours.
步骤三、在常压和氮气流量为100~400mL/min的条件下，将干燥后的块状物料加热至1000~1200℃，保温3~5h，随炉冷却至室温~100℃，出炉，得到钒氮合金。Step 3. Under the conditions of normal pressure and nitrogen flow rate of 100-400mL/min, heat the dried bulk material to 1000-1200°C, keep it warm for 3-5h, cool it to room temperature-100°C with the furnace, and take it out of the furnace to obtain Vanadium nitrogen alloy.
所述碳质还原剂为碳黑。The carbonaceous reducing agent is carbon black.
所述碳质还原剂的粒度为0.074~0.125mm。The particle size of the carbonaceous reducing agent is 0.074-0.125mm.
所述硫酸氧钒的粒度为0.074~0.125mm。The particle size of the vanadyl sulfate is 0.074-0.125mm.
本实施例制备的钒氮合金经测定：钒含量为78.12~80.43wt%；氮含量为12.82~14.87wt%；表观密度为3.06~3.36g/cm3。The vanadium-nitrogen alloy prepared in this embodiment is measured: the vanadium content is 78.12-80.43wt%, the nitrogen content is 12.82-14.87wt%, and the apparent density is 3.06-3.36g/cm 3 .
实施例2Example 2
一种钒氮合金的制备方法。本实施例除碳质还原剂，其余同实施例1。A preparation method of a vanadium nitrogen alloy. The present embodiment except carbonaceous reducing agent, all the other are the same as embodiment 1.
所述碳质还原剂为石墨和活性炭的混合物。The carbonaceous reducing agent is a mixture of graphite and activated carbon.
本实施例制备的钒氮合金经测定：钒含量为78.56~79.47wt%；氮含量为12.67~14.92wt%；表观密度为3.12~3.41g/cm3。The vanadium-nitrogen alloy prepared in this example is measured: the vanadium content is 78.56-79.47wt%, the nitrogen content is 12.67-14.92wt%, and the apparent density is 3.12-3.41g/cm 3 .
实施例3Example 3
一种钒氮合金的制备方法。本实施例采用的技术方案的具体步骤是：A preparation method of a vanadium nitrogen alloy. The concrete steps of the technical solution adopted in this embodiment are:
步骤一、将碳质还原剂和以无水物计的硫酸氧钒按质量比为(0.2~0.3)∶1配料，混匀，得到混合物料。Step 1: The carbonaceous reducing agent and vanadyl sulfate calculated as anhydrous matter are mixed according to the mass ratio of (0.2-0.3): 1, and mixed to obtain a mixed material.
步骤二、将所述混合物料机压为块状物料，所述块状物料的密度为1.6~1.9g/cm3；再将所述块状物料在60~120℃条件下干燥1~7h。Step 2: press the mixed material into a block material with a density of 1.6-1.9 g/cm 3 ; then dry the block material at 60-120°C for 1-7 hours.
步骤三、在常压和氮气流量为200~500mL/min的条件下，将干燥后的块状物料加热至1200~1300℃，保温2~4h，随炉冷却至室温~100℃，出炉，得到钒氮合金。Step 3. Under the conditions of normal pressure and nitrogen flow rate of 200-500mL/min, heat the dried bulk material to 1200-1300°C, keep it warm for 2-4h, cool it to room temperature-100°C with the furnace, and take it out of the furnace to obtain Vanadium nitrogen alloy.
所述碳质还原剂为石墨。The carbonaceous reducing agent is graphite.
所述碳质还原剂的粒度为0.125~0.250mm。The particle size of the carbonaceous reducing agent is 0.125-0.250 mm.
所述硫酸氧钒的粒度为0.125~0.250mm。The particle size of the vanadyl sulfate is 0.125-0.250mm.
本实施例制备的钒氮合金经测定：钒含量为77.92~79.73wt%；氮含量为13.65~16.92wt%；表观密度为3.09~3.45g/cm3。The vanadium-nitrogen alloy prepared in this example is measured: the vanadium content is 77.92-79.73wt%, the nitrogen content is 13.65-16.92wt%, and the apparent density is 3.09-3.45g/cm 3 .
实施例4Example 4
一种钒氮合金的制备方法。本实施例除碳质还原剂，其余同实施例3。A preparation method of a vanadium nitrogen alloy. The present embodiment except carbonaceous reducing agent, all the other are the same as embodiment 3.
所述碳质还原剂为碳黑和活性炭中的混合物。The carbonaceous reducing agent is a mixture of carbon black and activated carbon.
本实施例制备的钒氮合金经测定：钒含量为77.89~79.98wt%；氮含量为14.51~15.99wt%；表观密度为3.06~3.47g/cm3。The vanadium-nitrogen alloy prepared in this example is measured: the vanadium content is 77.89~79.98wt%, the nitrogen content is 14.51~15.99wt%, and the apparent density is 3.06~3.47g/cm 3 .
实施例5Example 5
一种钒氮合金的制备方法。本实施例采用的技术方案的具体步骤是：A preparation method of a vanadium nitrogen alloy. The concrete steps of the technical solution adopted in this embodiment are:
步骤一、将碳质还原剂和以无水物计的硫酸氧钒按质量比为(0.15~0.25)∶1配料，混匀，得到混合物料。Step 1. The carbonaceous reducing agent and the vanadyl sulfate calculated as anhydrous matter are mixed according to the mass ratio of (0.15-0.25): 1, and mixed to obtain a mixed material.
步骤二、将所述混合物料机压为块状物料，所述块状物料的密度为1.7~2.0g/cm3；再将所述块状物料在60~120℃条件下干燥1~7h。Step 2: press the mixed material into a block material with a density of 1.7-2.0 g/cm 3 ; then dry the block material at 60-120° C. for 1-7 hours.
步骤三、在常压和氮气流量为300~600mL/min的条件下，将干燥后的块状物料加热至1300~1400℃，保温1~3h，随炉冷却至室温~100℃，出炉，得到钒氮合金。Step 3. Under the conditions of normal pressure and nitrogen flow rate of 300-600mL/min, heat the dried bulk material to 1300-1400°C, keep it warm for 1-3h, cool it to room temperature-100°C with the furnace, and take it out of the furnace to obtain Vanadium nitrogen alloy.
所述碳质还原剂为活性炭。The carbonaceous reducing agent is activated carbon.
所述碳质还原剂的粒度为0.100~0.175mm。The particle size of the carbonaceous reducing agent is 0.100-0.175 mm.
所述硫酸氧钒的粒度为0.100~0.175mm。The particle size of the vanadyl sulfate is 0.100-0.175mm.
本实施例制备的钒氮合金经测定：钒含量为77.52~79.86wt%；氮含量为15.31~16.98wt%；表观密度为3.10~3.46g/cm3。The vanadium-nitrogen alloy prepared in this example is measured: the vanadium content is 77.52-79.86wt%, the nitrogen content is 15.31-16.98wt%, and the apparent density is 3.10-3.46g/cm 3 .
实施例6Example 6
一种钒氮合金的制备方法。本实施例除碳质还原剂，其余同实施例5。A preparation method of a vanadium nitrogen alloy. The present embodiment except carbonaceous reductant, all the other are the same as embodiment 5.
所述碳质还原剂为碳黑和石墨的混合物。The carbonaceous reducing agent is a mixture of carbon black and graphite.
本实施例制备的钒氮合金经测定：钒含量为77.81~79.62wt%；氮含量为14.39~16.91wt%；表观密度为3.03~3.54g/cm3。The vanadium-nitrogen alloy prepared in this example is measured: the vanadium content is 77.81-79.62wt%, the nitrogen content is 14.39-16.91wt%, and the apparent density is 3.03-3.54g/cm 3 .
实施例7Example 7
一种钒氮合金的制备方法。本实施例除碳质还原剂，其余同实施例5。A preparation method of a vanadium nitrogen alloy. The present embodiment except carbonaceous reductant, all the other are the same as embodiment 5.
所述碳质还原剂为碳黑、石墨和活性炭中的混合物。The carbonaceous reducing agent is a mixture of carbon black, graphite and activated carbon.
本实施例制备的钒氮合金经测定：钒含量为78.12~79.89wt%；氮含量为14.76~16.03wt%；表观密度为3.11~3.48g/cm3。The vanadium-nitrogen alloy prepared in this embodiment is measured: the vanadium content is 78.12-79.89wt%, the nitrogen content is 14.76-16.03wt%, and the apparent density is 3.11-3.48g/cm 3 .
本具体实施方式的有益效果是：The beneficial effect of this embodiment is:
(1)本具体实施方式采用硫酸氧钒作为原料，由于硫酸氧钒含有结晶水和吸附水，在造块过程中无需外加粘结剂，工艺简单。(1) This specific embodiment adopts vanadyl sulfate as a raw material. Since vanadyl sulfate contains crystal water and adsorption water, no additional binder is needed in the agglomeration process, and the process is simple.
(2)本具体实施方式采用的硫酸氧钒在加热过程中分解，使得物料的比表面积增大，增加了与氮气的接触面积，提高了还原氮化速率，增加了氮含量，无需外加促进剂且还原氮化时间短。(2) The vanadyl sulfate adopted in this specific embodiment is decomposed in the heating process, so that the specific surface area of the material is increased, the contact area with nitrogen is increased, the reduction nitriding rate is improved, the nitrogen content is increased, and no additional accelerator is required And the reduction and nitriding time is short.
(3)本具体实施方式反应温度低，有利于节约能耗。(3) The reaction temperature of this specific embodiment is low, which is conducive to saving energy consumption.
本具体实施方式制备的钒氮合金经检测：钒含量为77.52~80.43wt%；氮含量为12.67~16.98wt%；表观密度为3.03~3.54g/cm3。The vanadium-nitrogen alloy prepared in this embodiment is tested: the vanadium content is 77.52-80.43wt%, the nitrogen content is 12.67-16.98wt%, and the apparent density is 3.03-3.54g/cm 3 .
因此，本具体实施方式具有工艺简单、反应时间短和反应温度低的特点。Therefore, this specific embodiment has the characteristics of simple process, short reaction time and low reaction temperature.
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