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A technology of metal and rhenium powder, which is applied in the field of preparing metal rhenium, can solve problems such as increased process costs, achieve the effects of increasing specific surface area and surface energy, uniform particle shape, and improving activity
Active Publication Date: 2019-02-01
洛阳双罗铼材料科技有限公司
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This method decomposes ammonium rhenate into Re 2 o 7 In the process, it can partially reduce the impurity doping in the hydrogen reduction process and improve the purity of the metal rhenium powder. However, in the implementation process of this method, oxygen, carrier gas and reducing gas need to be used respectively, and the carrier gas N 2 or Ar will contain Re 2 o 7 The gaseous product of the gaseous product is transported to the reduction zone and then reduced, the carrier gas will 2 o 7 Concentration produces dilution, which increases process cost
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Embodiment 1
[0043] Raw material: high-purity ammonium perrhenate, purity 99.96%;
[0044] Implementation process:
[0045] The first step is to prepare high-purity ultrafine ammonium perrhenate;
[0046] 1) Add the raw materials into pure water at 60°C at a solid-to-liquid ratio of 140g:1L, stir until completely dissolved, adjust the pH to 8~9 with ammonia water, and slowly add H at a ratio of 0.5mL / g 2 o 2 , stop heating and filtering until there are no bubbles, and cool the filtrate to room temperature;
[0047] 2) Introduce the filtrate into the ultrasonic crystallizer, conduct ultrasonic crystallization at 2°C for 1 hour, and the ultrasonic power of the ultrasonic crystallizer is 1000W; Ultrasonic vibrating plate, the ultrasonic vibrating plate is set at the bottom of the kettle body and fixed on the mounting hole of the thermal insulation plate through the fixing rod, and can be disassembled freely;
[0048] 3) After the crystallization is completed, drain, dehydrate, and vacuum ...
Embodiment 2
[0053] Raw material: crude ammonium perrhenate, purity 99.50%;
[0054] Implementation process:
[0055] The first step is to prepare high-purity ultrafine ammonium perrhenate;
[0056] Add the raw materials into pure water at 80°C at a solid-to-liquid ratio of 160g:1L, stir until completely dissolved, adjust the pH to 8~9 with ammonia water, and slowly add H at a ratio of 2mL / g. 2 o 2 , stop heating and filtering until there are no bubbles, and cool the filtrate to room temperature;
[0057] 2) Introduce the filtrate into the ultrasonic crystallizer, conduct ultrasonic crystallization at 0~1°C for 3 hours, and the ultrasonic power of the ultrasonic crystallizer is 2000W; The device uses 5 ultrasonic vibrating rods, and the top of each ultrasonic vibrating rod is fixed on the corresponding 5 mounting holes on the thermal insulation board through connecting rods, and can be disassembled freely;
[0058] 3) After the crystallization is completed, drain, dehydrate, and vacuum...
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Abstract
The invention relates to the technical field of rhenium recycling and use, in particular to a method for preparing metallic rhenium. According to the method provided by the invention, the high-purity metallic rhenium is prepared by taking ammonium perrhenate as a raw material through two steps; in the first step, high-purity ultrafine ammonium perrhenate is first prepared; in the second step, the ammonium perrhenate is reduced into high-purity metallic rhenium powder through a reducing method; ultrasonic auxiliary crystallization and vacuum drying are adopted; in the process of ultrasonic crystallization, an ultrasonic crystallizer with an opened kettle body and a detachable ultrasonic transducer are adopted. Due to the adoption of an ultrasonic crystallization-hydrogen reduction combined process, the ammonium perrhenate serving as the raw material is used for preparing the high-purity metallic rhenium, so that the flow is simplified, the reaction time is shortened, the energy is saved, and the consumption is reduced; the raw material is high in adaptability, so that the requirement on the raw material is lowered; ultrasonic waves directly act on the ammonium perrhenate material, and the utilization rate is high; the detachable structure is easy to check and replace, and favorable for industrialization.
Description
technical field [0001] The invention relates to the technical field of rhenium industry, in particular to a method for preparing metal rhenium. Background technique [0002] Rhenium (Re) is a kind of dispersed refractory metal. Due to its excellent physical and chemical properties, rhenium and its compounds are widely used in the aerospace industry, instrument industry and electronic and electrical functional materials. [0003] The high temperature resistance of rhenium has led to its use in heating elements, electrical plugs, thermocouples, special wires and components in electronic tubes, so the consumption of electronic materials has increased. Rhenium is mainly used with tungsten, molybdenum, nickel, niobium, etc. Metal alloys are used in electronic components, high-temperature thermocouples and electrode materials (WO2004 / 070748, WO2008041540A1, EP2221839A2), and due to the high melting point of rhenium metal, powder metallurgy is generally used to process rhenium-cont...
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