CN104999073B - A kind of metal vapors reduction prepares the method and device of high-purity low-oxygen titanium valve - Google Patents
A kind of metal vapors reduction prepares the method and device of high-purity low-oxygen titanium valve Download PDFInfo
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 120
- 238000000034 method Methods 0.000 title claims abstract description 51
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 50
- 239000002184 metal Substances 0.000 title claims abstract description 50
- 239000001301 oxygen Substances 0.000 title claims abstract description 27
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 27
- 230000009467 reduction Effects 0.000 title claims abstract description 14
- 239000010936 titanium Substances 0.000 title claims description 43
- 229910052719 titanium Inorganic materials 0.000 title claims description 42
- 238000010438 heat treatment Methods 0.000 claims abstract description 27
- 239000000463 material Substances 0.000 claims abstract description 24
- 238000000889 atomisation Methods 0.000 claims description 23
- 238000005984 hydrogenation reaction Methods 0.000 claims description 21
- 238000006356 dehydrogenation reaction Methods 0.000 claims description 19
- 239000002994 raw material Substances 0.000 claims description 15
- 238000006722 reduction reaction Methods 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 12
- -1 titanium hydride Chemical compound 0.000 claims description 11
- 229910000048 titanium hydride Inorganic materials 0.000 claims description 11
- 239000012535 impurity Substances 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 10
- 239000011261 inert gas Substances 0.000 claims description 7
- 238000005868 electrolysis reaction Methods 0.000 claims description 6
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- 229910044991 metal oxide Inorganic materials 0.000 claims description 2
- 150000004706 metal oxides Chemical class 0.000 claims description 2
- 238000005554 pickling Methods 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 claims 1
- 229910052739 hydrogen Inorganic materials 0.000 claims 1
- 239000002923 metal particle Substances 0.000 claims 1
- 238000002791 soaking Methods 0.000 claims 1
- 238000004140 cleaning Methods 0.000 abstract 1
- 230000007613 environmental effect Effects 0.000 abstract 1
- 235000021110 pickles Nutrition 0.000 abstract 1
- 150000003839 salts Chemical class 0.000 description 19
- 230000008569 process Effects 0.000 description 13
- 238000006243 chemical reaction Methods 0.000 description 7
- 239000007789 gas Substances 0.000 description 7
- 238000009689 gas atomisation Methods 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 238000009413 insulation Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 229910000831 Steel Inorganic materials 0.000 description 4
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- 229920000742 Cotton Polymers 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 229910018068 Li 2 O Inorganic materials 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
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Abstract
本发明公开了一种金属蒸气还原制备高纯低氧钛粉的方法及装置，该方法包括采用一种金属蒸气还原制备高纯低氧钛粉的方法及装置，将活泼金属和钛粉置于真空密封加热炉中进行金属蒸气还原制得高纯钛粉，然后对高纯钛粉进行水洗、酸洗和干燥得到高纯低氧钛粉的步骤；该装置包括具有炉腔的炉体，炉腔的中部设有炉膛，炉膛内设有炉罐，炉罐中放置有料框，料框上装设有筛网，筛网与炉罐的底部之间留有间距，炉罐的顶部开口端密封连接有可拆卸的炉盖，炉盖上设有排气阀、压力表和抽真空管道，炉罐还连接有进气管。本发明具有成本低、效率高、环保清洁等优点。
The invention discloses a method and a device for preparing high-purity low-oxygen titanium powder by metal vapor reduction. The method comprises a method and a device for preparing high-purity low-oxygen titanium powder by metal vapor reduction. Carry out metal vapor reduction in a vacuum-sealed heating furnace to obtain high-purity titanium powder, and then wash, pickle and dry the high-purity titanium powder to obtain high-purity low-oxygen titanium powder; the device includes a furnace body with a furnace cavity, a furnace There is a furnace in the middle of the cavity, and a furnace tank is arranged in the furnace tank. A material frame is placed in the furnace tank, and a screen is installed on the material frame. There is a distance between the screen and the bottom of the furnace tank, and the top open end of the furnace tank is sealed and connected There is a detachable furnace cover, which is equipped with an exhaust valve, a pressure gauge and a vacuum pipe, and the furnace tank is also connected with an air inlet pipe. The invention has the advantages of low cost, high efficiency, environmental protection and cleaning.
Description
技术领域technical field
本发明涉及粉末制备技术领域，具体涉及一种金属蒸气还原制备高纯低氧钛粉的方法及装置。The invention relates to the technical field of powder preparation, in particular to a method and a device for preparing high-purity low-oxygen titanium powder by metal vapor reduction.
背景技术Background technique
作为新兴金属的一员，钛拥有许多优秀的特性，如比强度大、比重小、耐腐蚀等，而纯钛一般指的是纯度大于99%的钛材料。高纯钛具有许多优良的性能，如密度低、熔点高、强度低、塑性好等特点，近年来，随着航空航天、电子信息等高科技产业的快速发展，高纯钛的用量也越来越多，如何更好地制备高纯钛，是当今钛工业发展的重要方向。As a member of emerging metals, titanium has many excellent properties, such as high specific strength, small specific gravity, corrosion resistance, etc., and pure titanium generally refers to titanium materials with a purity greater than 99%. High-purity titanium has many excellent properties, such as low density, high melting point, low strength, and good plasticity. In recent years, with the rapid development of high-tech industries such as aerospace and electronic information, the amount of high-purity titanium is also increasing. How to better prepare high-purity titanium is an important direction for the development of today's titanium industry.
目前制备高纯钛粉最常用的方法主要为氢化脱氢或雾化法，但经过氢化脱氢或雾化法制得纯度高的钛粉，其氧含量较高，其中氢化脱氢得到的钛粉为不规则形状；而雾化法得到的钛粉虽为球形，但雾化过程中容易发生粉末颗粒粘连，粉末粒度偏大并且粒径分布很宽，故需要进一步的提纯得到高纯低氧的钛粉。例如，以采用海绵钛作为原料，通过氢化脱氢制备得到高纯钛粉为例，由于海绵钛杂质含量偏高，且与高温下极易发生氧化形成TiO2引入主要杂质O元素，最后制得的钛粉的杂质含量（尤其是氧含量）较高，严重影响了最终制得钛粉的性能，不能满足工业要求；同时，粉末在高温脱氢阶段中也容易长大和结块，因此钛粉的纯度和粒度很难达到理想的程度，严重制约了粉末冶金钛行业的发展。At present, the most commonly used method for preparing high-purity titanium powder is mainly hydrogenation dehydrogenation or atomization method, but the high-purity titanium powder obtained by hydrogenation dehydrogenation or atomization method has a high oxygen content, and the titanium powder obtained by hydrogenation dehydrogenation Irregular shape; and the titanium powder obtained by the atomization method is spherical, but the powder particles are prone to sticking during the atomization process, the powder particle size is too large and the particle size distribution is very wide, so further purification is required to obtain high-purity and low-oxygen titanium powder. Titanium powder. For example, take titanium sponge as a raw material and prepare high-purity titanium powder by hydrogenation dehydrogenation as an example. Due to the high impurity content of titanium sponge and the high temperature, it is easy to oxidize to form TiO 2 to introduce the main impurity O element, and finally produce The impurity content (especially the oxygen content) of the titanium powder is high, which seriously affects the performance of the final titanium powder and cannot meet the industrial requirements; at the same time, the powder is also easy to grow and agglomerate in the high-temperature dehydrogenation stage, so the titanium powder It is difficult to achieve the ideal level of purity and particle size, which seriously restricts the development of powder metallurgy titanium industry.
发明内容Contents of the invention
本发明要解决的技术问题是克服现有技术存在的不足，提供一种成本低、效率高、环保清洁的金属蒸气还原制备高纯低氧钛粉的方法及装置。The technical problem to be solved by the present invention is to overcome the deficiencies in the prior art and provide a low-cost, high-efficiency, environmentally friendly and clean method and device for preparing high-purity low-oxygen titanium powder by metal vapor reduction.
为解决上述技术问题，本发明采用以下技术方案：In order to solve the problems of the technologies described above, the present invention adopts the following technical solutions:
一种金属蒸气还原制备高纯低氧钛粉的方法，其特征在于：包括以下步骤：A method for preparing high-purity low-oxygen titanium powder by metal vapor reduction, characterized in that: comprising the following steps:
（1）选取高纯度熔盐电解钛为原料，采用氢化脱氢或雾化法对熔盐电解钛加工制得钛粉；(1) Select high-purity molten salt electrolytic titanium as raw material, and use hydrogenation dehydrogenation or atomization to process molten salt electrolytic titanium to obtain titanium powder;
（2）将重量相同的活泼金属和钛粉置于真空密封加热炉中，在真空环境下加热至使活泼金属形成蒸气，活泼金属蒸气与钛粉中的杂质发生还原反应得到高纯钛粉；其中，钛粉中的主要杂质TiO2被还原，从而得到高纯Ti粉；(2) Put the active metal and titanium powder of the same weight in a vacuum sealed heating furnace, and heat in a vacuum environment until the active metal forms vapor, and the active metal vapor and the impurities in the titanium powder undergo a reduction reaction to obtain high-purity titanium powder; Among them, TiO2 , the main impurity in titanium powder, is reduced to obtain high-purity Ti powder;
（3）对高纯钛粉进行水洗、酸洗和干燥去除附着的金属氧化物，得到高纯低氧钛粉。(3) Washing, pickling and drying the high-purity titanium powder to remove attached metal oxides to obtain high-purity low-oxygen titanium powder.
上述的方法，优选的，钛粉与活泼金属非直接接触地置于真空密封加热炉中。在还原过程中，钛粉与活泼金属不直接接触，该种方式避免了直接接触造成的产物污染问题，利于降低产品中杂质的含量。In the above method, preferably, the titanium powder is placed in a vacuum-sealed heating furnace in non-direct contact with the active metal. During the reduction process, the titanium powder does not directly contact the active metal. This method avoids the product pollution caused by direct contact and is beneficial to reduce the content of impurities in the product.
上述的方法，优选的，所述步骤（2）中，活泼金属制备成颗粒置于真空密封加热炉内料框的的底部，钛粉通过筛网放置在活泼金属颗粒的上方。In the above method, preferably, in the step (2), the active metal is prepared into granules and placed at the bottom of the material frame in the vacuum-sealed heating furnace, and the titanium powder is placed above the active metal granules through a screen.
上述的方法，优选的，所述步骤（2）中，加热温度为1273~1290K，保温时间为2~3小时，所述真空密封加热炉内的真空度为3.3×10-3Pa~8.2×10-3Pa。In the above method, preferably, in the step (2), the heating temperature is 1273~1290K, the holding time is 2~3 hours, and the vacuum degree in the vacuum sealed heating furnace is 3.3×10 -3 Pa~8.2× 10 -3 Pa.
上述的方法，优选的，所述活泼金属为Na，K，Ca，Li或Mg。In the above method, preferably, the active metal is Na, K, Ca, Li or Mg.
上述的方法，优选的，所述活泼金属和钛粉的加入量均为50~60g。In the above method, preferably, the active metal and titanium powder are added in an amount of 50-60 g.
上述的方法，优选的，所述氢化脱氢法对熔盐电解钛加工包括氢化、球磨和脱氢三个步骤，具体是，先将原料置于氢化脱氢炉中氢化得到氢化钛颗粒，再将氢化钛颗粒球磨破碎得到氢化钛粉末，然后将氢化钛粉末置于氢化脱氢炉中脱氢制得钛粉；所述雾化法对熔盐电解钛加工包括惰性气体雾化法和旋转电极雾化法。其中，惰性气体雾化法即借助高速气流来击碎金属液流；旋转电极雾化法即用金属或合金制作成一对电极，通过放电使得金属端面与电弧接触区域变成熔融状态，再通过高速旋转的离心力将金属液滴甩出，完成雾化过程。In the above method, preferably, the hydrodehydrogenation method includes three steps of hydrogenation, ball milling and dehydrogenation for molten salt electrolytic titanium processing. Specifically, the raw materials are first placed in a hydrodehydrogenation furnace for hydrogenation to obtain titanium hydride particles, and then Titanium hydride particles are ball milled to obtain titanium hydride powder, and then the titanium hydride powder is placed in a hydrogenation dehydrogenation furnace to dehydrogenate to obtain titanium powder; the atomization method includes inert gas atomization method and rotating electrode for molten salt electrolytic titanium processing Atomization method. Among them, the inert gas atomization method uses high-speed airflow to crush the metal liquid flow; the rotating electrode atomization method uses metal or alloy to make a pair of electrodes, and the contact area between the metal end surface and the arc becomes molten through discharge, and then through high-speed The centrifugal force of the rotation throws the metal droplets out to complete the atomization process.
本发明中，高纯熔盐电解钛为颗粒状。In the present invention, the high-purity molten salt electrolytic titanium is in granular form.
作为一个总的发明构思，本发明还提供一种用于金属蒸气还原制备高纯低氧钛粉的装置，包括具有炉腔的炉体，所述炉腔的中部设有炉膛，所述炉膛内设有炉罐，所述炉罐中放置有料框，所述料框上装设有筛网，所述筛网与炉罐的底部之间留有间距，所述炉罐的顶部开口端密封连接有可拆卸的炉盖，所述炉盖上设有排气阀、压力表和抽真空管道，所述炉罐还连接有进气管。As a general inventive concept, the present invention also provides a device for preparing high-purity low-oxygen titanium powder by metal vapor reduction, comprising a furnace body with a furnace chamber, a furnace chamber is provided in the middle of the furnace chamber, and A retort is provided, a material frame is placed in the retort, a screen is installed on the material frame, a distance is left between the screen and the bottom of the retort, and the top open end of the retort is sealed and connected with A detachable furnace cover is provided with an exhaust valve, a pressure gauge and a vacuuming pipeline, and the furnace tank is also connected with an air inlet pipe.
上述的装置，优选的，所述炉盖通过压紧装置密封安装于炉罐上；所述进气管上设有流量计。For the above-mentioned device, preferably, the furnace cover is sealed and installed on the furnace tank through a pressing device; a flow meter is provided on the inlet pipe.
上述的装置，优选的，所述炉膛与炉体内壁之间填充有保温棉。For the above-mentioned device, preferably, insulation cotton is filled between the furnace hearth and the inner wall of the furnace.
上述的装置，优选的，所述炉体、炉膛、炉罐、料框和炉盖均由不锈钢制成。For the above device, preferably, the furnace body, furnace hearth, furnace tank, material frame and furnace cover are all made of stainless steel.
上述的装置，优选的，所述筛网表面分布有多个圆形气孔，这种圆形气孔能使气体通过而不让钛粉掉落。In the above-mentioned device, preferably, a plurality of circular air holes are distributed on the surface of the screen, and the circular air holes can allow gas to pass through without dropping the titanium powder.
上述的装置，优选的，所述炉盖升降由电动丝杆升降机完成，且壳体由型钢和钢板焊接成型，炉盖衬采用全纤维结构，保温性能好。For the above-mentioned device, preferably, the lifting of the furnace cover is completed by an electric screw lifter, and the shell is welded and formed by section steel and steel plate, and the furnace cover lining adopts a full-fiber structure, which has good thermal insulation performance.
上述的装置，在实验时，将用于产生金属蒸气的活泼金属置于料框底部，被还原钛粉置于料框的筛网上，然后关闭炉盖，即可用于实验。抽取真空后开始加热至一定温度并保温一段时间，产生的金属蒸气通过筛网的气孔与被还原钛粉接触，发生还原反应，从而避免了活泼金属和被还原钛粉直接接触造成的产物污染问题。此外，可拆卸的炉盖与炉体密封连接，起到了保障炉体密封性的作用，避免了密封状态下的气体逸出，保证了炉膛内部足量的压强，从而确保还原反应正确高效地进行，也避免了炉内气体逸出所造成的环境污染问题，同时，也避免了炉外气体进入炉内造成的反应干扰问题。For the above-mentioned device, during the experiment, the active metal used to generate metal vapor is placed at the bottom of the material frame, the reduced titanium powder is placed on the screen of the material frame, and then the furnace cover is closed, which can be used for the experiment. After vacuuming, start heating to a certain temperature and keep it warm for a period of time. The metal vapor generated will contact the reduced titanium powder through the pores of the screen, and a reduction reaction will occur, thereby avoiding the product pollution caused by the direct contact between the active metal and the reduced titanium powder. . In addition, the detachable furnace cover is sealed and connected with the furnace body, which plays a role in ensuring the sealing of the furnace body, avoids the escape of gas in the sealed state, and ensures sufficient pressure inside the furnace, thereby ensuring that the reduction reaction is carried out correctly and efficiently , It also avoids the problem of environmental pollution caused by the escape of gas in the furnace, and at the same time, it also avoids the problem of reaction interference caused by the gas outside the furnace entering the furnace.
上述装置在实验时，随着反应温度的不断升高，炉内气体的压力不断升高，浓度增大，加热到一定温度并保温的过程中，活泼金属蒸气能够充分地与筛网上的被还原金属发生反应，确保反应高效地进行。整个装置具有强度高、可重复使用、结构简单、成本低、密闭性优良、操作方法简单等特点。During the experiment of the above-mentioned device, with the continuous increase of the reaction temperature, the pressure of the gas in the furnace is continuously increased, and the concentration is increased. During the process of heating to a certain temperature and keeping it warm, the active metal vapor can be fully combined with the reduced gas on the screen. The metal reacts to ensure that the reaction proceeds efficiently. The whole device has the characteristics of high strength, reusability, simple structure, low cost, excellent airtightness, simple operation method and the like.
与现有技术相比，本发明的优点在于：本发明金属蒸气还原制备高纯低氧钛粉的方法以高纯熔盐电解钛为原料，采用氢化脱氢法或雾化法结合金属蒸气还原工艺制备高纯低氧钛粉，其在原料及提纯工艺上均进行了创新。首先，原料选择上，选取高纯熔盐电解钛为原料，其成分中氧含量低（约为100ppm），杂质含量极少（约为500ppm)，且所用原料不涉及高污染生产工艺，环保清洁。其次，通过氢化脱氢或雾化法得到的钛粉，虽然氧含量较高，但其它杂质含量较少，有利于最终得到高纯低氧钛粉。通过金属蒸气还原钛粉工艺最终得到的钛粉氧含量低（小于1000ppm），其它杂质含量也极低（小于100ppm），且粒度细小，工艺性能优良。该制备方法的成本低、效率高，造成的污染也很少，所得产品可广泛应用于粉末冶金净成型加工、耐磨耐蚀部件、涂料制备等行业。Compared with the prior art, the present invention has the advantages that: the method for preparing high-purity low-oxygen titanium powder by metal vapor reduction in the present invention uses high-purity molten salt electrolytic titanium as raw material, adopts hydrogenation dehydrogenation method or atomization method combined with metal vapor reduction The process prepares high-purity low-oxygen titanium powder, which has made innovations in raw materials and purification processes. First of all, in the selection of raw materials, high-purity molten salt electrolytic titanium is selected as the raw material. The oxygen content in the composition is low (about 100ppm), and the impurity content is very small (about 500ppm). The raw materials used do not involve high-pollution production processes, and are environmentally friendly and clean. . Secondly, although the titanium powder obtained by hydrogenation dehydrogenation or atomization method has a high oxygen content, it has low content of other impurities, which is beneficial to finally obtain high-purity low-oxygen titanium powder. The final titanium powder obtained by metal vapor reduction titanium powder process has low oxygen content (less than 1000ppm), and extremely low content of other impurities (less than 100ppm), and has fine particle size and excellent process performance. The preparation method has low cost, high efficiency and little pollution, and the obtained product can be widely used in industries such as powder metallurgy net shape processing, wear-resistant and corrosion-resistant parts, coating preparation and the like.
附图说明Description of drawings
图1为本发明用于金属蒸气还原制备高纯低氧钛粉的装置的结构示意图。Fig. 1 is a schematic structural view of the device for preparing high-purity low-oxygen titanium powder by metal vapor reduction according to the present invention.
图例说明：illustration:
1、炉体；2、炉膛；3、炉罐；4、料框；5、筛网；6、炉盖；7、排气阀；8、压力表；9、抽真空管道；10、进气管；11、压紧装置；12、流量计；13、保温棉；14、电控柜。1. Furnace body; 2. Furnace chamber; 3. Furnace tank; 4. Material frame; 5. Screen; 6. Furnace cover; 7. Exhaust valve; 8. Pressure gauge; ; 11. Compression device; 12. Flow meter; 13. Thermal insulation cotton; 14. Electric control cabinet.
具体实施方式detailed description
以下结合附图和具体实施例对本发明作进一步详细说明。The present invention will be described in further detail below in conjunction with the accompanying drawings and specific embodiments.
实施例1：Example 1:
选取高纯熔盐电解钛为原料，采用氢化脱氢法对熔盐电解钛加工制得钛粉；将50g氢化脱氢得到的钛粉放入真空密封加热炉内料框的筛网上，选用Ca作为还原金属，在真空密封加热炉料框底部加入50gCa，抽取真空至真空密封加热炉内真空度达到8.2×10-3Pa后密封，然后在真空环境下升温加热至1278K并保温2h，反应完成后得到高纯钛粉，待冷却至室温后，通过对高纯钛粉进行水洗、酸洗和干燥除去附着在高纯钛粉上的CaO，得到高纯低氧钛粉。Select high-purity molten salt electrolytic titanium as raw material, and use hydrogenation dehydrogenation method to process molten salt electrolysis titanium to obtain titanium powder; put 50g of titanium powder obtained by hydrogenation dehydrogenation into the screen of the material frame in the vacuum-sealed heating furnace, select Ca As a reduced metal, add 50g Ca at the bottom of the vacuum-sealed heating furnace material frame, pump the vacuum until the vacuum degree in the vacuum-sealed heating furnace reaches 8.2×10 -3 Pa, seal it, and then heat it up to 1278K in a vacuum environment and keep it for 2 hours. After the reaction is completed The high-purity titanium powder is obtained. After cooling to room temperature, the high-purity titanium powder is washed with water, pickled and dried to remove CaO attached to the high-purity titanium powder to obtain high-purity low-oxygen titanium powder.
实施例2：Example 2:
选取高纯熔盐电解钛为原料，采用雾化法对熔盐电解钛加工制得钛粉；将60g惰性气体雾化法得到的钛粉放入真空密封加热炉内料框的筛网上，选用Na作为还原金属，在真空密封加热炉料框底部加入60gNa，抽取真空至真空密封加热炉内真空度达到8.2×10-3Pa后密封，然后在真空环境下升温加热至1285K并保温3h，反应完成后得到高纯钛粉，待冷却至室温后，通过对高纯钛粉进行水洗、酸洗和干燥除去附着在高纯钛粉上的Na2O，得到高纯低氧钛粉。Select high-purity molten salt electrolytic titanium as the raw material, and use the atomization method to process the molten salt electrolytic titanium to obtain titanium powder; put 60g of titanium powder obtained by the inert gas atomization method into the screen of the material frame in the vacuum-sealed heating furnace, and select Na is used as a reducing metal, add 60g Na to the bottom of the vacuum-sealed heating furnace material frame, pump the vacuum until the vacuum degree in the vacuum-sealed heating furnace reaches 8.2×10 -3 Pa, seal it, then raise the temperature to 1285K in a vacuum environment and keep it warm for 3 hours, the reaction is completed Finally, high-purity titanium powder is obtained. After cooling to room temperature, the high-purity titanium powder is washed with water, pickled and dried to remove Na 2 O attached to the high-purity titanium powder to obtain high-purity low-oxygen titanium powder.
实施例3：Example 3:
选取高纯熔盐电解钛为原料，采用雾化法对熔盐电解钛加工制得钛粉；将60g旋转电极雾化法得到的钛粉放入真空密封加热炉内料框的筛网上，选用K作为还原金属，在真空密封加热炉料框底部加入60gK，抽取真空至真空密封加热炉内真空度达到8.2×10-3Pa后密封，然后在真空环境下升温加热至1273K并保温2h，反应完成得到高纯钛粉，待冷却至室温后，通过对高纯钛粉进行水洗、酸洗和干燥除去附着在高纯钛粉上的K2O，得到高纯低氧钛粉。Select high-purity molten salt electrolytic titanium as the raw material, and use the atomization method to process the molten salt electrolytic titanium to obtain titanium powder; put 60g of titanium powder obtained by the rotating electrode atomization method into the screen of the inner material frame of the vacuum-sealed heating furnace, and select K is used as a reducing metal, add 60g K to the bottom of the vacuum-sealed heating furnace material frame, pump the vacuum until the vacuum degree in the vacuum-sealed heating furnace reaches 8.2×10 -3 Pa, seal it, then raise the temperature to 1273K in a vacuum environment and keep it warm for 2 hours, the reaction is completed The high-purity titanium powder is obtained, and after being cooled to room temperature, the high-purity titanium powder is washed with water, pickled and dried to remove K 2 O attached to the high-purity titanium powder to obtain high-purity low-oxygen titanium powder.
实施例4：Example 4:
选取高纯熔盐电解钛为原料，采用氢化脱氢法对熔盐电解钛加工制得钛粉；将55g氢化脱氢得到的钛粉放入真空密封加热炉内料框的筛网上，选用Li作为还原金属，在真空密封加热炉料框底部加入55gLi，抽取真空至真空密封加热炉内真空度达到8.2×10-3Pa后密封，然后在真空环境下升温加热至1288K并保温2h，反应完成后得到高纯钛粉，待冷却至室温后，通过对高纯钛粉进行水洗、酸洗和干燥除去附着在得到高纯钛粉上的Li2O，得到高纯低氧钛粉。Select high-purity molten salt electrolytic titanium as raw material, and use hydrogenation dehydrogenation method to process molten salt electrolysis titanium to obtain titanium powder; put 55g of titanium powder obtained by hydrogenation dehydrogenation into the screen of the material frame in the vacuum-sealed heating furnace, select Li As a reduced metal, add 55gLi to the bottom of the vacuum-sealed heating furnace material frame, pump the vacuum until the vacuum degree in the vacuum-sealed heating furnace reaches 8.2×10 -3 Pa, seal it, then heat it up to 1288K in a vacuum environment and keep it warm for 2 hours. After the reaction is completed The obtained high-purity titanium powder is cooled to room temperature, and the high-purity titanium powder is washed with water, pickled and dried to remove Li 2 O attached to the obtained high-purity titanium powder to obtain high-purity low-oxygen titanium powder.
实施例5：Example 5:
选取高纯熔盐电解钛为原料，采用雾化法对熔盐电解钛加工制得钛粉；将50g等离子旋转电极雾化法得到的钛粉放入真空密封加热炉内料框的筛网上，选用Mg作为还原金属，在真空密封加热炉料框底部加入50gMg，抽取真空至真空密封加热炉内真空度达到8.2×10-3Pa后密封，然后在真空环境下升温加热至1275K并保温2h，反应完成后得到高纯钛粉，待冷却至室温后，通过对高纯钛粉进行水洗、酸洗和干燥除去附着在高纯钛粉上的MgO，即可得到高纯低氧钛粉。Select high-purity molten salt electrolytic titanium as the raw material, and use the atomization method to process the molten salt electrolytic titanium to obtain titanium powder; put 50g of titanium powder obtained by the plasma rotating electrode atomization method into the screen of the material frame in the vacuum-sealed heating furnace, Select Mg as the reducing metal, add 50g of Mg to the bottom of the vacuum-sealed heating furnace material frame, draw the vacuum until the vacuum degree in the vacuum-sealed heating furnace reaches 8.2×10 -3 Pa, seal it, then raise the temperature to 1275K in a vacuum environment and keep it warm for 2h, and react After completion, high-purity titanium powder is obtained. After cooling to room temperature, the high-purity titanium powder is washed with water, pickled and dried to remove MgO attached to the high-purity titanium powder, and high-purity low-oxygen titanium powder can be obtained.
上述实施例1至5中，氢化脱氢法对熔盐电解钛加工包括氢化、球磨和脱氢三个步骤，具体是，先将原料置于氢化脱氢炉中氢化得到氢化钛颗粒，再将氢化钛颗粒球磨破碎得到氢化钛粉末，然后将氢化钛粉末置于氢化脱氢炉中脱氢制得钛粉；雾化法对熔盐电解钛加工包括惰性气体雾化法和旋转电极雾化法，惰性气体雾化法和旋转电极雾化法均为现有技术，其中，惰性气体雾化法即借助高速气流来击碎金属液流；旋转电极雾化法即用金属或合金制作成一对电极，通过放电使得金属端面与电弧接触区域变成熔融状态，再通过高速旋转的离心力将金属液滴甩出，完成雾化过程。In the above-mentioned Examples 1 to 5, the hydrogenation dehydrogenation method includes three steps of hydrogenation, ball milling and dehydrogenation for the processing of molten salt electrolytic titanium. Titanium hydride particles are crushed by ball milling to obtain titanium hydride powder, and then the titanium hydride powder is placed in a hydrogenation dehydrogenation furnace to dehydrogenate to obtain titanium powder; the atomization method includes inert gas atomization method and rotating electrode atomization method for molten salt electrolytic titanium processing , the inert gas atomization method and the rotating electrode atomization method are both existing technologies, wherein the inert gas atomization method uses a high-speed air flow to crush the metal liquid flow; the rotating electrode atomization method uses a metal or alloy to make a pair of electrodes , the contact area between the metal end face and the arc becomes molten through discharge, and then the metal droplets are thrown out by the centrifugal force of high-speed rotation to complete the atomization process.
实施例6：Embodiment 6:
如图1所示，一种用于金属蒸气还原制备高纯低氧钛粉的装置，包括具有炉腔的炉体1，炉腔的中部设有炉膛2，炉膛2内设有炉罐3，炉罐3中放置有料框4，料框4上装设有筛网5，筛网5与炉罐3的底部之间留有间距，炉罐3的顶部开口端密封连接有可拆卸的炉盖6，炉盖6上设有排气阀7、压力表8和抽真空管道9，炉罐3还连接有进气管10。As shown in Figure 1, a kind of device that is used for the reduction of metal vapor to prepare high-purity low-oxygen titanium powder comprises a body of furnace 1 with a furnace cavity, the middle part of the furnace cavity is provided with a furnace 2, and a retort 3 is arranged in the furnace 2, A material frame 4 is placed in the retort 3, and a screen 5 is installed on the material frame 4. There is a distance between the screen 5 and the bottom of the retort 3. The top open end of the retort 3 is sealed and connected with a detachable furnace cover 6. , The furnace cover 6 is provided with an exhaust valve 7, a pressure gauge 8 and a vacuum pipe 9, and the retort 3 is also connected with an intake pipe 10.
本实施例中，炉盖6通过压紧装置11密封安装于炉罐3上，在其他实施例中，炉盖6也可以采用螺钉、螺栓等方式与炉罐3连接；进气管10上设有流量计12。In this embodiment, the furnace cover 6 is sealed and installed on the retort 3 through the pressing device 11. In other embodiments, the furnace cover 6 can also be connected with the retort 3 by means of screws, bolts, etc.; flowmeter12.
本实施例中，炉膛2与炉体1内壁之间填充有保温棉13。炉体1的外壁上设有电控柜14。In this embodiment, insulation cotton 13 is filled between the furnace hearth 2 and the inner wall of the furnace body 1 . An electric control cabinet 14 is provided on the outer wall of the furnace body 1 .
本实施例中，炉体1、炉膛2、炉罐3、料框4和炉盖6均由不锈钢制成。筛网5为表面分布有多个圆形气孔的板，这种圆形气孔能使气体通过而不让钛粉掉落。炉盖6升降进一步可由电动丝杆升降机完成，且壳体由型钢和钢板焊接成型，炉盖衬采用全纤维结构，保温性能好。In this embodiment, the furnace body 1, the furnace chamber 2, the furnace tank 3, the material frame 4 and the furnace cover 6 are all made of stainless steel. The screen cloth 5 is a plate with a plurality of circular air holes distributed on the surface, and this circular air hole can allow the gas to pass through without allowing the titanium powder to drop. The lifting of the furnace cover 6 can be further completed by an electric screw lifter, and the shell is formed by welding steel and steel plates, and the furnace cover lining adopts a full-fiber structure with good thermal insulation performance.
以上所述仅是本发明的优选实施方式，本发明的保护范围并不仅局限于上述实施例。对于本技术领域的技术人员来说，在不脱离本发明技术构思前提下所得到的改进和变换也应视为本发明的保护范围。The above descriptions are only preferred implementations of the present invention, and the scope of protection of the present invention is not limited to the above examples. For those skilled in the art, improvements and transformations obtained without departing from the technical concept of the present invention should also be regarded as the protection scope of the present invention.
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