A kind of method of vacuum refining purification of crude selenium material

A vacuum refining and raw material technology, applied in the direction of binary selenium/tellurium compounds, elemental selenium/tellurium, etc., can solve the problems of poor field operation environment, low output of single equipment, and low-grade selenium products, so as to achieve good working environment, Effect of reducing product contamination and increasing density

Active Publication Date: 2019-08-20
KUNMING DIBOO TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The present invention provides a method for vacuum refining and purifying crude selenium materials, aiming at the problems of long purification process flow of crude selenium materials, poor on-site operating environment, low output of a single device, and low-grade selenium products produced.

Method used

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  • A kind of method of vacuum refining purification of crude selenium material

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Experimental program
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Effect test

Embodiment 1

[0039] Step 1, 300Kg copper electrolytic anode slime is processed the crude selenium material produced in the process of recycling gold and silver (the main components are: selenium 92.35%, tellurium 0.01%, lead 0.73%, water 0.29%, other is copper, iron and other salts class) into the closed melting electric furnace at one time, and the electric furnace is heated up to 230° C. to melt the crude selenium material. After the crude selenium material in the electric furnace is completely melted, the electric furnace is heated to 260°C for degassing. During the degassing process, the melting electric furnace is vacuumed with a water circulation pump, and the vacuum degree of the melting electric furnace is kept at 500-4000Pa. The selenium melt was stirred for 2 hours to obtain a density of 4.2 g / cm 3 crude selenium melt.

[0040] Step 2. Put the melted and degassed crude selenium melt into a graphite crucible, place the graphite crucible in a vacuum distillation furnace, and vacuu...

Embodiment 2

[0043] Step 1, 500Kg copper electrolytic anode slime is processed the crude selenium material (main composition is: selenium 82.7%, tellurium 0.87%, lead 1.18%, water 28.53%, other is copper, iron and other salt ) at a speed of 14g / s stably added in the airtight melting electric furnace, and the electric furnace was slowly heated to 300° C. to melt the crude selenium material. When melting, a vacuum pump was used to evacuate the melting electric furnace while constantly stirring the crude selenium material. After the 500Kg crude selenium material in the closed melting electric furnace is completely melted, the electric furnace is heated to 350°C for degassing. During the degassing process, a vacuum pump is used to vacuum the melting electric furnace. While stirring the selenium melt, stirring for 1 hour to obtain a density of 4.5g / cm 3 crude selenium melt.

[0044] Step 2. The crude selenium melt melted and degassed in step 1 is released from the discharge port of the closed ...

Embodiment 3

[0048] Step 1, 650Kg copper electrolytic anode slime is processed the crude selenium material (main components are: selenium 76.04%, tellurium 5.08%, lead 8.78%, water 28.12%, other is copper, iron and other salt class) at a rate of 30Kg once per 20 minutes into the closed electric furnace for melting, and after the initial feeding, the electric furnace is heated to 350°C to melt the crude selenium material, and at the same time, the crude selenium material is continuously stirred. After 650Kg of crude selenium materials are all put into the airtight melting electric furnace, and the material is completely melted, the electric furnace is heated to 400°C for degassing. During the degassing process, the melting electric furnace is vacuumed with a vacuum pump, and the vacuum degree of the melting electric furnace is controlled to 2000-10000Pa. At the same time, the selenium melt was stirred, and after stirring for 0.5 hours, the obtained density was 4.8g / cm 3 crude selenium melt....

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Abstract

The invention relates to a vacuum refining and purifying method for a coarse selenium material and belongs to the field of metallurgy technological engineering. The method is characterized in that a fine selenium product is obtained from the coarse selenium material through procedures of smelting, degassing and vacuum distillation. The method specifically comprises the following steps: S1, adding the coarse selenium material into a closed container to be smelted at 230-350 DEG C; after the material is fully smelted, raising the temperature to 250-400 DEG C to degas, vacuumizing the closed container during degassing, and stirring the selenium melt at the same time to obtain a coarse selenium melt, the density of which is greater than 4g / cm<3>; and S2, putting the coarse selenium melt obtained in the S1 into a vacuum furnace, and distilling the coarse selenium melt for 3-4 hours to output a fine selenium product, wherein the vacuum degree is 1-20Pa and the temperature is 500-1000 DEG C. The method provided by the invention is short in process flow, and 99.9% of fine selenium can be output from the coarse selenium material through procedures of smelting, degassing and vacuum distillation.

Description

technical field [0001] The invention relates to the field of metallurgical technology engineering, in particular to a method for vacuum refining and purifying crude selenium materials. Background technique [0002] Selenium is an important semiconductor material with a melting point of 221°C and a boiling point of 685°C. The abundance of selenium in the earth's crust is only 0.05-0.09mg / kg, and no single selenium deposit with economic value has been found in nature. Selenium is usually associated with metal sulfide ores such as copper, lead, and nickel. The main source of selenium is the by-products produced during the smelting of heavy metal sulfide ores, while the amount of selenium produced from copper electrolytic anode slime and copper sulfide ore smelting dust accounts for about 90% of the total selenium output, and the rest comes from the refining output of lead, cobalt and nickel It is recovered from the calcine and the acid mud produced by sulfuric acid and the was...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B19/02C01B19/04
Inventor 戴卫平速斌陈巍汤文通潘建仁杨斌李红陈浩杨堃余勇朱坤红杨寿云
Owner KUNMING DIBOO TECH
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