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Equipment and method for preparing high-purity tellurium

A technology for high-purity tellurium and equipment, which is applied in the field of industrialized preparation of high-purity tellurium, can solve the problems of poor tellurium purification effect, high energy consumption, low distillation efficiency, etc. Effect

Active Publication Date: 2020-03-20
CENT SOUTH UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When the temperature rises from 500°C to 550°C, the difference between the saturated vapor pressure of impurity elements and tellurium is more obvious. If the distillation temperature continues to increase, the ratio of the difference between impurity elements and saturated vapor pressure will decrease, which is not conducive to the separation of tellurium and impurities and affects the separation of tellurium. The purification effect
[0013] Master's thesis "Research on the Purification of Tellurium by Vacuum Distillation-Zone Melting, Liu Siqi" discloses a tower-type vacuum distillation tellurium purification furnace. The product is easy to block the pipeline and other problems
CN201720015085.X discloses a vacuum distillation device for refining high-purity metals. Although it can be purified and prepared for high-purity metals, the device is a one-stage distillation device, and the purification effect for metal raw materials with many types of impurities is poor. The bottom of the device is an inverted trapezoid Raw material kettle, low distillation efficiency and long cycle
CN 201720594376.9 discloses a device for preparing high-purity gallium by distillation and separation. The device has a good purification effect on gallium and high evaporation efficiency, but the device is designed according to the nature of gallium and is not suitable for the purification of tellurium. In addition, the device has poor controllability and no cooling system The temperature control accuracy is not high, and it is impossible to monitor the evaporation inside the distillation device
[0014] CN201110439767.0 discloses a high-purity selenium preparation equipment and method, the device can prepare 6N high-purity selenium, but the device adopts the traditional charging method, and the distillation efficiency is low; the device is designed according to the properties of selenium and is not suitable for Selenium and other impurities with a saturated vapor pressure similar to metal tellurium are separated, and the purification effect of tellurium is poor; the device uses a traditional coil temperature controller, and the temperature control accuracy in the distillation process is low; the device has no observation hole and cannot monitor the vacuum distillation process; The material outlet is not equipped with a heating device, and the residual material is easy to cool and block the outlet, which affects the normal operation of the distillation process
CN 201110456181.5 discloses a high-purity selenium preparation equipment and method. The device can prepare 5N high-purity zinc. The device has problems such as low distillation efficiency, low temperature control accuracy, and inability to monitor the purity of the distillation product in real time. In addition, the method is based on zinc The nature of the design, not suitable for vacuum distillation of tellurium
CN 201821265882.4 discloses a large-scale equipment for preparing high-purity tellurium pellets. Although the batch preparation of high-purity tellurium pellets can be realized, the device can only shape the tellurium material, and cannot realize the efficient purification of tellurium, and the raw material adaptability is poor
[0015] Therefore, the currently disclosed high-purity tellurium or high-purity tellurium preparation devices are still difficult to solve the problems of low distillation efficiency, poor distillation temperature control precision, and poor removal of impurities in tellurium metal in the large-scale production of high-purity tellurium by vacuum distillation of tellurium. , Unable to monitor the distillation process in real time and long process, high production cost, high energy consumption, low preparation efficiency and other issues

Method used

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  • Equipment and method for preparing high-purity tellurium
  • Equipment and method for preparing high-purity tellurium
  • Equipment and method for preparing high-purity tellurium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0073] Evenly place 5 kg of crude tellurium raw material with a purity of 5N in a clean 6-layer graphite retort 39, record the data displayed by the weight sensor 20, fix and seal the sampling monitoring tube 19, graphite tray 41, collecting funnel 38 and distillation top in sequence. Cover 5, open single-hole vacuum suction filter 23 and double-hole vacuum suction filter 9 to carry out vacuum treatment, vacuum still 3, molten metal buffer kettle 8, hydrogen reduction furnace 11 and each molten metal feeding pipe 7 that is connected are in a vacuum state. Wait for the vacuum degree to reach 8×10 -3 After pa, turn on the high-frequency heating device for heating, control the internal heating temperature of the vacuum distillation kettle 3 to about 500°C, and keep the temperature of the conical condenser 36 and the vertical sampling detection tube 19 at 270°C for 4 hours. During this process, the crude tellurium raw material gradually melts, and The impurity elements whose satu...

Embodiment 2

[0083] Evenly place 5 kg of crude tellurium raw material with a purity of 5N in a clean 6-layer graphite retort 39, record the data displayed by the weight sensor, fix and seal the sampling monitoring tube 19, graphite tray 41, collecting funnel 38 and distillation top cover in sequence 5, open the single-hole vacuum suction filter 23 and the double-hole vacuum suction filter 9 to carry out vacuum treatment, the vacuum still 3, the molten metal buffer kettle 8, the hydrogen reduction furnace 11 and each molten metal feeding pipe 7 connected in a vacuum. Wait for the vacuum degree to reach 9×10 -3 After pa, turn on the high-frequency heating device to heat, control the internal heating temperature of the vacuum distillation kettle 3 to about 505°C, and the temperature of the conical condenser 36 and the vertical sampling detection tube 19 to be 273°C for 4 hours. During this process, the tellurium raw material gradually melts and becomes saturated. The impurity elements whose ...

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Abstract

The invention discloses equipment and a method for preparing high-purity tellurium. The equipment comprises a vacuum distillation device, a vacuumizing device, a hydrogen purification circulating device, a high-frequency induction heating device and a product collecting device; the vacuumizing device is used for providing a vacuum environment and comprises a single-hole vacuum suction filter and adouble-hole vacuum suction filter, and the single-hole vacuum suction filter is connected with an extraction opening in a vacuum distillation kettle; and the hydrogen purification circulating deviceis used for providing a hydrogen reduction environment for the product collecting device. When the equipment is used for preparing high-purity tellurium, the process is short, the energy consumption is low, the tellurium remelting procedure in the conventional high-purity tellurium preparation process is omitted, and the problems of high energy consumption caused in the remelting process and localoxidation caused in the charging process are avoided.

Description

technical field [0001] The invention relates to a technology for preparing high-purity tellurium, in particular to an equipment and method for industrially preparing high-purity tellurium. Background technique [0002] The atomic number of tellurium in the periodic table is 52, which is located between selenium and polonium in the main group VI of the fifth cycle. Compared with sulfur and selenium, it has more obvious metallic properties. With the continuous development of today's science and technology, the rapid progress of metallurgy, especially the iron and steel industry and military and other cutting-edge technology fields, the requirements for the purity of tellurium are becoming more and more stringent, and the demand is increasing. At present, the methods for preparing high-purity tellurium include zone smelting method, chemical method, vacuum distillation method, etc. However, it is difficult to increase the purity of tellurium to 6N by purely chemical method, so i...

Claims

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Application Information

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IPC IPC(8): C01B19/02
CPCC01B19/02Y02P10/20
Inventor 郭学益张磊田庆华李栋许志鹏
Owner CENT SOUTH UNIV
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