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Method for producing high-purity selenium through ultrasonic enhanced reduction

An ultrasonic strengthening, high-purity selenium technology, applied in the field of materials, can solve the problems of long processing cycle, high risk of flue gas pollution to the atmospheric environment, and low selenium purity.

Active Publication Date: 2021-06-04
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, the selenium purification processes reported at home and abroad mainly include crude selenium oxidation and volatilization method, hydrogen selenide pyrolysis method, ion exchange method, zone smelting method, and vacuum distillation method. Among them, the crude selenium oxidation and volatilization method has a long process and low yield. , SeO 2 The risk of flue gas polluting the atmospheric environment is high, and industrial application is difficult to implement; hydrogen selenide pyrolysis can produce extremely pure selenium (99.9997%), but hydrogen selenide is highly toxic, and it is impossible to realize industrialization with existing technical equipment ; The saturation capacity of the adsorption material of the ion exchange method is limited, the material cost is high, and the adsorption material needs to be regenerated, and the operating cost is high; the regional smelting method has strict requirements on the composition of the raw material, the processing cycle is long, the cost is high, and the yield is low. It is not suitable for large-scale production; when the vacuum distillation method is used to purify crude selenium materials, the Se-Te separation effect is not good, and the purity of the obtained selenium is not high, and further wet treatment is required

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  • Method for producing high-purity selenium through ultrasonic enhanced reduction
  • Method for producing high-purity selenium through ultrasonic enhanced reduction
  • Method for producing high-purity selenium through ultrasonic enhanced reduction

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment 1: a kind of method that ultrasonic enhancement reduction produces high-purity selenium (see figure 1 ),Specific steps are as follows:

[0025] (1) Selenium oxide is obtained through cascade inert microwave distillation to obtain high-purity selenium oxide; wherein, in terms of mass percentage, the main impurity element content of high-purity zinc oxide is 20.8ppm, and the distillation atmosphere is argon, and the first time of cascade inert distillation The distillation temperature is 300°C and the time is 5 minutes, which can realize a large amount of separation of easy-to-handle selenium oxide and impurities; the second distillation temperature is 500°C and the time is 1 minute, so as to realize the deep separation of residual selenium oxide and impurities;

[0026] In terms of mass percentage, the components of selenium oxide raw materials are shown in Table 1, and the components of high-purity selenium oxide are shown in Table 2,

[0027] Table 1 seleni...

Embodiment 2

[0037] Embodiment 2: a kind of method that supersonic enhanced reduction produces high purity selenium (see figure 1 ),Specific steps are as follows:

[0038] (1) Selenium oxide is subjected to cascade inert microwave distillation to obtain high-purity selenium oxide; wherein, in terms of mass percentage, the main impurity element content of high-purity zinc oxide is 14.9 ppm, and the distillation atmosphere is argon, and the first time of cascade inert distillation The distillation temperature is 300°C and the time is 5 minutes, which can realize a large amount of separation of easy-to-handle selenium oxide and impurities; the second distillation temperature is 500°C and the time is 1 minute, so as to realize the deep separation of residual selenium oxide and impurities;

[0039] In terms of mass percentage, the components of selenium oxide raw materials are shown in Table 4, and the components of high-purity selenium oxide are shown in Table 5,

[0040] Table 4 selenium oxi...

Embodiment 3

[0050] Embodiment 3: a kind of method (see figure 1 ),Specific steps are as follows:

[0051] (1) Selenium oxide is subjected to cascade inert microwave distillation to obtain high-purity selenium oxide; wherein, in terms of mass percentage, the main impurity element content of high-purity zinc oxide is 9.6ppm, and the distillation atmosphere is nitrogen, and the first distillation of the cascade inert distillation The temperature is 500°C, and the time is 30 minutes, which can realize a large amount of separation of easy-to-handle selenium oxide and impurities; the second distillation temperature is 700°C, and the time is 15 minutes, so as to realize the deep separation of residual selenium oxide and impurities;

[0052] In terms of mass percentage, the components of selenium oxide raw materials are shown in Table 7, and the components of high-purity selenium oxide are shown in Table 8,

[0053] Table 7 selenium oxide raw material impurity components (ppm)

[0054]

[00...

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Abstract

The invention relates to a method for producing high-purity selenium through ultrasonic enhanced reduction, and belongs to the technical field of materials. The method comprises the following steps: carrying out cascade inert distillation on selenium oxide to obtain high-purity selenium oxide, dissolving the high-purity selenium oxide in dilute sulfuric acid to obtain a seleninic acid solution, carrying out ultrasonic enhanced reduction reaction on the seleninic acid solution, carrying out solid-liquid separation, and washing and drying the solid to obtain high-purity selenium. According to the method, local stirring is enhanced by utilizing reducibility. H generated by ultrasound and a high-temperature and high-pressure environment, a larger reduction potential is achieved, seleninic acid is reduced to generate high-purity selenium, the production cost of the high-purity selenium is low, the purity of the obtained selenium is high, and operation conditions are friendly.

Description

technical field [0001] The invention relates to a method for producing high-purity selenium through ultrasonic enhanced reduction, belonging to the technical field of materials. Background technique [0002] With the continuous development and progress of science and technology, high-purity selenium plays an increasingly indispensable and important role in many fields, especially high-tech industrial sectors, such as semiconductor equipment, optoelectronic equipment, selenium solar cells, lasers and infrared light guides and so on. As an important main material or auxiliary material, high-purity selenium plays an increasingly important role in the national economy, and the market demand continues unabated. [0003] At present, the selenium purification processes reported at home and abroad mainly include crude selenium oxidation and volatilization method, hydrogen selenide pyrolysis method, ion exchange method, zone smelting method, and vacuum distillation method. Among the...

Claims

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Application Information

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IPC IPC(8): C01B19/02
CPCC01B19/02
Inventor 张利波杨坤王天潘锡剑洪岩曾翰林
Owner KUNMING UNIV OF SCI & TECH
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